CN117680083B - Preparation process and preparation device of tetrakis (hydroxymethyl) phosphonium sulfate - Google Patents
Preparation process and preparation device of tetrakis (hydroxymethyl) phosphonium sulfate Download PDFInfo
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- CN117680083B CN117680083B CN202410155666.8A CN202410155666A CN117680083B CN 117680083 B CN117680083 B CN 117680083B CN 202410155666 A CN202410155666 A CN 202410155666A CN 117680083 B CN117680083 B CN 117680083B
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- preparation
- formaldehyde
- sulfuric acid
- solution
- tetrakis
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- 238000002360 preparation method Methods 0.000 title claims abstract description 125
- YIEDHPBKGZGLIK-UHFFFAOYSA-L tetrakis(hydroxymethyl)phosphanium;sulfate Chemical compound [O-]S([O-])(=O)=O.OC[P+](CO)(CO)CO.OC[P+](CO)(CO)CO YIEDHPBKGZGLIK-UHFFFAOYSA-L 0.000 title claims abstract description 57
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 215
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 195
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims abstract description 92
- 239000011259 mixed solution Substances 0.000 claims abstract description 55
- 238000005507 spraying Methods 0.000 claims abstract description 55
- 239000000243 solution Substances 0.000 claims abstract description 48
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims abstract description 46
- 239000007864 aqueous solution Substances 0.000 claims abstract description 41
- 238000003756 stirring Methods 0.000 claims abstract description 40
- 239000008098 formaldehyde solution Substances 0.000 claims abstract description 38
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims description 57
- 238000006243 chemical reaction Methods 0.000 claims description 42
- 239000007789 gas Substances 0.000 claims description 40
- 230000007246 mechanism Effects 0.000 claims description 40
- 238000001125 extrusion Methods 0.000 claims description 38
- 238000007599 discharging Methods 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000007921 spray Substances 0.000 claims description 12
- 238000002347 injection Methods 0.000 claims description 10
- 239000007924 injection Substances 0.000 claims description 10
- 238000010521 absorption reaction Methods 0.000 claims description 6
- 238000009792 diffusion process Methods 0.000 claims description 5
- ZGTNBBQKHJMUBI-UHFFFAOYSA-N bis[tetrakis(hydroxymethyl)-lambda5-phosphanyl] sulfate Chemical compound OCP(CO)(CO)(CO)OS(=O)(=O)OP(CO)(CO)(CO)CO ZGTNBBQKHJMUBI-UHFFFAOYSA-N 0.000 claims description 3
- LMFWXTZEFKLNSB-UHFFFAOYSA-N OS(O)(=O)=O.OS(O)(=O)=O.OS(O)(=O)=O.P.P Chemical compound OS(O)(=O)=O.OS(O)(=O)=O.OS(O)(=O)=O.P.P LMFWXTZEFKLNSB-UHFFFAOYSA-N 0.000 abstract description 7
- 230000035515 penetration Effects 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract 1
- 230000004927 fusion Effects 0.000 description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- -1 at the moment Substances 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000013013 elastic material Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- CBOIHMRHGLHBPB-UHFFFAOYSA-N hydroxymethyl Chemical compound O[CH2] CBOIHMRHGLHBPB-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/54—Quaternary phosphonium compounds
- C07F9/5407—Acyclic saturated phosphonium compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/002—Nozzle-type elements
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention discloses a preparation process and a preparation device of tetrakis (hydroxymethyl) phosphonium sulfate, and relates to the technical field of the preparation of the tetrakis (hydroxymethyl) phosphonium sulfate. The invention includes a preparation column; the mixing and stirring part comprises a formaldehyde inlet pipe fixedly arranged on the preparation tower and used for feeding formaldehyde solution; s1, when the preparation of the aqueous solution of the tetrakis (hydroxymethyl) phosphonium sulfate is carried out, firstly, formaldehyde solution and sulfuric acid solution are respectively injected into a preparation tower through a formaldehyde inlet pipe and a sulfuric acid inlet pipe according to the mol ratio of 8:1. The advantages are that: the invention can fully mix the formaldehyde solution and the sulfuric acid solution by adopting the mode of rotating and stirring and matching with reciprocating swing and penetration, and fully contact and react the formaldehyde solution and the sulfuric acid solution with phosphine gas in a constant-temperature environment by adopting the mode of spraying offer, thereby effectively improving the contact range and the contact time between the formaldehyde and sulfuric acid mixed solution and the phosphine gas and having higher overall preparation efficiency of the tetra-methylol phosphorus sulfate aqueous solution.
Description
Technical Field
The invention relates to the technical field of preparation of tetrakis (hydroxymethyl) phosphonium sulfate, in particular to a preparation process and a preparation device of the tetrakis (hydroxymethyl) phosphonium sulfate.
Background
The tetra-methylol phosphorus sulfate is a weak alkaline colorless transparent liquid, is a novel, efficient and excellent bactericide, can also be used as a permanent flame retardant for pure cotton and polyester cotton fabrics, and is generally prepared by adopting a tetra-methylol phosphorus sulfate preparation device;
The Chinese patent application No. CN201110057949.1 discloses a preparation method of tetrakis (hydroxymethyl) phosphonium sulfate, which comprises the following steps: adding sulfuric acid and formaldehyde into a reaction kettle, opening a gas-liquid circulation mixing reaction pump, adding phosphine into the gas-liquid circulation mixing reaction pump, absorbing phosphine at 50-60 ℃ through the gas-liquid circulation mixing reaction device, enabling the phosphine which is not completely absorbed to enter the next gas-liquid circulation mixing reaction pump, detecting the content of formaldehyde through central control, judging the end point of the reaction, and concentrating under reduced pressure after the reaction is finished to obtain the tetrakis (hydroxymethyl) phosphonium sulfate. The invention has the advantages of simplicity, low cost, capability of improving the reaction speed by about 40%, no blockage of equipment, simple equipment installation and operation, and suitability for industrial production of waste gas recycling;
the above device still has the following disadvantages:
1. When the device is used for preparing the tetrakis (hydroxymethyl) phosphonium sulfate, only a simple pouring mode is adopted for mixing formaldehyde and sulfuric acid solution, the formaldehyde and sulfuric acid solution cannot be fully mixed in the mixing mode, the fusion property of the formaldehyde and the sulfuric acid solution is poor, and the follow-up high-efficiency reaction with phosphine gas is not facilitated;
2. When the device is used for preparing the tetra-methylol phosphorus sulfate, the formaldehyde and sulfuric acid solution are injected into the phosphine gas for mixed reaction, and the injection mode can lead the contact range between the phosphine gas and the formaldehyde and sulfuric acid solution to be smaller, the overall reaction time to be longer, and the preparation efficiency of the tetra-methylol phosphorus sulfate aqueous solution to be lower;
Therefore, there is a need to design a process and a device for preparing the tetrakis (hydroxymethyl) phosphonium sulfate to solve the above problems.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation process and a preparation device of tetrakis (hydroxymethyl) phosphonium sulfate, which solve the problems in the prior art.
In order to achieve the above purpose, the invention is realized by the following technical scheme: a preparation process of a preparation device of tetrakis (hydroxymethyl) phosphonium sulfate comprises a preparation tower;
The mixing and stirring part comprises a formaldehyde inlet pipe for feeding formaldehyde solution, which is fixedly arranged on a preparation tower, a sulfuric acid inlet pipe for feeding sulfuric acid solution is fixedly arranged on the preparation tower, a servo motor is fixedly arranged at the bottom of the preparation tower, a driving roller is fixedly arranged on the driving end of the servo motor, and a stirring mechanism is arranged on the driving roller, the stirring mechanism comprises a driven roller fixedly arranged on the driving roller, an electric self-locking wheel I is matched with the driven roller, a plurality of fixing frames are fixedly arranged on the electric self-locking wheel I, a self-resetting rotating roller is rotatably arranged on each fixing frame, a plurality of stirring rods are fixedly arranged on each self-resetting rotating roller, and a collecting arc disc for bearing formaldehyde solution and sulfuric acid solution is fixedly arranged in the preparation tower;
The solution spraying part is used for enabling formaldehyde and sulfuric acid mixed solution to rapidly and uniformly spray downwards, the solution spraying part comprises a spraying box fixedly arranged at the lower part of the collecting arc disc, an extrusion mechanism is arranged between the driving roller and the spraying box, the extrusion mechanism comprises an extrusion disc arranged in the spraying box through a sliding limiting structure, an electric self-locking wheel II is arranged on the driven roller in a matched mode, a reciprocating screw rod is fixedly arranged on the electric self-locking wheel II, a ball nut is arranged on the reciprocating screw rod in a matched mode, the ball nut is fixedly connected with the extrusion disc, and a liquid discharging structure is arranged between the collecting arc disc and the spraying box;
The liquid discharging structure comprises a plurality of liquid discharging pipes fixedly communicated between the spraying box and the collecting arc disc, and a plurality of spraying holes are formed in the lower part of the spraying box;
the absorption reaction part is used for carrying out rapid reaction of phosphine gas, formaldehyde and sulfuric acid mixed solution to prepare a tetrakis hydroxymethyl phosphonium sulfate aqueous solution, the absorption reaction part comprises two linkage rollers rotatably arranged on a preparation tower, a linkage mechanism is arranged between the two linkage rollers and the driving roller, the linkage mechanism comprises an electric self-locking wheel III fixedly arranged on the driving roller, a driving bevel gear is fixedly arranged on the electric self-locking wheel III, driven bevel gears are fixedly arranged on the two linkage rollers, and the two driven bevel gears are meshed with the driving bevel gear;
The two linkage rollers are provided with a scooping mechanism, the scooping mechanism comprises a fixed wheel fixedly arranged on the linkage rollers, a plurality of scooping spoons are fixedly arranged on the fixed wheel, and the back side of each scooping spoon is fixedly provided with a temperature control heating plate for heating;
The preparation tower is internally and fixedly provided with a reaction disc, the reaction disc is provided with arc grooves matched with a plurality of scooping and dispersing spoons, the arc grooves are used for bearing a tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution, the preparation tower is provided with an air inlet mechanism for the air inlet of phosphine gas, the air inlet mechanism comprises an accessory barrel fixedly arranged on the preparation tower, the air outlet end of the air pump is fixedly provided with an upper air pipe, a plurality of air injection pipes are fixedly arranged between the upper air pipe and the preparation tower, the preparation tower is internally provided with a collecting mechanism, the collecting mechanism comprises a bearing disc fixedly arranged on the preparation tower, the reaction disc is fixedly provided with a plurality of liquid passing pipes, and the preparation tower is fixedly provided with a collecting pipe matched with the bearing disc;
the preparation process applied to the preparation device comprises the following steps:
S1, when the preparation of the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution is carried out, firstly, injecting formaldehyde solution and sulfuric acid solution into a preparation tower according to the mol ratio of the formaldehyde inlet pipe to the sulfuric acid inlet pipe, and accumulating the formaldehyde solution and the sulfuric acid solution on a collecting arc disc in the preparation tower;
s2, restarting the servo motor to drive the driving roller and the driven roller to rotate, starting the electric self-locking wheel I to enable the driving roller and the driven roller to jointly rotate, and enabling the electric self-locking wheel I to rotate so as to drive stirring rods in a plurality of stirring mechanisms to synchronously rotate, so that formaldehyde solution and sulfuric acid solution can be fully stirred to be uniformly mixed;
s3, after the formaldehyde solution and the sulfuric acid solution are stirred and mixed, a plurality of liquid discharging pipes can be opened to enable the mixed solution to enter the lower part of an extrusion disc in the spraying box through the liquid discharging pipes and be accumulated, and transfer of the formaldehyde solution and the sulfuric acid solution is completed;
s4, restarting the second electric self-locking wheel to lock the second electric self-locking wheel with the driven roller, starting the servo motor to drive the driving roller, the driven roller and the second electric self-locking wheel to rotate, so as to drive the reciprocating screw rod to rotate, namely, driving the extrusion disc to reciprocate up and down under the cooperation of the ball nut, and extruding the mixed solution at the lower part of the extrusion disc in a reciprocating manner when the extrusion disc descends, so that the mixed solution is sprayed into the preparation tower in a reciprocating intermittent manner through a plurality of spraying holes;
S5, spraying the formaldehyde and sulfuric acid mixed solution, and simultaneously starting an air supply pump to spray phosphine gas in an accessory barrel into the preparation tower through an upper air pipe and a plurality of air injection pipes, wherein the phosphine gas and the formaldehyde and sulfuric acid mixed solution are fully contacted and reacted, and at the moment, a plurality of temperature control heating plates synchronously start heating the formaldehyde and sulfuric acid mixed solution, so that the temperature in the preparation tower is controlled between the degree and the degree, and the preparation work of the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution can be started;
s6, when the reaction is carried out, the electric self-locking wheel III is started to be locked with the driving roller, and the servo motor is started to drive the driving roller III to rotate, so that the driving bevel gear can be driven to rotate, and the two linkage rollers are driven to jointly rotate under the cooperation of the two driven bevel gears;
S7, the two linkage rollers rotate to drive the plurality of scooping and dispersing scoops to rotate under the cooperation of the fixed wheels, and when the scooping and dispersing scoops rotate, the formaldehyde and sulfuric acid mixed solution in the arc-shaped groove scoops up to be fully diffused in the preparation tower, so that the formaldehyde and sulfuric acid mixed solution can be fully contacted and reacted with phosphine gas, and the reaction efficiency is improved;
S8, after the mixed solution of formaldehyde and sulfuric acid reacts with phosphine gas, generating a tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution, stacking the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution in an arc-shaped groove on a reaction disc, opening a plurality of liquid passing pipes to enable the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution to fall into a bearing disc, and opening a collecting pipe to take out and collect the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution.
Preferably, each stirring rod is provided with a plurality of stirring holes.
Preferably, the plurality of liquid discharging pipes are in sliding connection with the extrusion disc, and an elastic taper ring is fixedly arranged on the inner wall of each spraying hole.
Preferably, the sliding limiting structure comprises a plurality of limiting sliding rods fixedly mounted on the extrusion disc, a plurality of limiting sliding grooves are formed in the inner wall of the spraying box, the limiting sliding rods are respectively clamped and slidably mounted in the corresponding limiting sliding grooves, and two limiting spring rods are fixedly mounted between the extrusion disc and the inner wall of the spraying box.
Preferably, each ladle is provided with a liquid containing tank, and a phosphine inlet pipe for feeding phosphine gas is fixedly arranged in the auxiliary tank.
Preferably, each air jet pipe is fixedly provided with an air jet diffusion cover.
Preferably, the liquid outlet ends of the liquid passing pipes are all positioned at the lower part of the bearing disc, and a plurality of liquid passing pipes, a plurality of air injection pipes, phosphine inlet pipes, a plurality of liquid discharging pipes, formaldehyde inlet pipes and sulfuric acid inlet pipes are all provided with control valves.
The invention provides a preparation process and a preparation device of tetrakis (hydroxymethyl) phosphonium sulfate. The beneficial effects are as follows:
1. When the preparation of the aqueous solution of the tetrakis (hydroxymethyl) phosphonium sulfate is carried out, the formaldehyde solution and the sulfuric acid solution can be fully and uniformly mixed by adopting a stirring mode of combining reciprocating swing and penetration while rotating and stirring a plurality of groups of stirring rods, so that the fusion of the formaldehyde solution and the sulfuric acid solution is stronger, and the preparation efficiency of the aqueous solution of the tetrakis (hydroxymethyl) phosphonium sulfate can be effectively improved.
2. When the preparation of the aqueous solution of the tetrakis (hydroxymethyl) phosphonium sulfate is carried out, the mixed solution of formaldehyde and sulfuric acid can be intermittently sprayed into the preparation tower by adopting a reciprocating intermittent spraying mode, so that the contact range and the contact time between the mixed solution of formaldehyde and sulfuric acid and phosphine gas can be effectively increased, and the reaction efficiency is further improved.
3. When the preparation of the aqueous solution of the tetra-methylol phosphorus sulfate is carried out, the mixed solution of the formaldehyde and the sulfuric acid is fully diffused and dispersed in the preparation tower by adopting a reciprocating scooping offer mode, so that the contact range and the contact time between the mixed solution of the formaldehyde and the sulfuric acid and phosphine gas can be further increased, and the preparation efficiency of the aqueous solution of the tetra-methylol phosphorus sulfate is effectively improved.
In summary, the formaldehyde solution and the sulfuric acid solution are fully mixed by adopting the mode of rotating and stirring and matching with reciprocating swing and penetration, and the formaldehyde solution and the sulfuric acid solution are fully contacted and reacted with phosphine gas in a constant-temperature environment by adopting the mode of spraying offer, so that the contact range and the contact time between the formaldehyde and sulfuric acid mixed solution and the phosphine gas can be effectively improved, and the overall preparation efficiency of the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution is higher.
Drawings
The invention is described in further detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a schematic diagram of a process and apparatus for preparing tetrakis (hydroxymethyl) phosphonium sulfate according to the present invention;
FIG. 2 is a cross-sectional view of the internal structure of FIG. 1;
FIG. 3 is an enlarged view showing the internal structure of the production tower of FIG. 1;
FIG. 4 is an enlarged view of the upper structure of the servo motor and the shower box of FIG. 3;
FIG. 5 is an enlarged view of the structure of the stirring mechanism of FIG. 4;
FIG. 6 is a cross-sectional view of the interior structure of the showerhead cartridge of FIG. 4;
FIG. 7 is a schematic view of the upper structure of the squeeze plate of FIG. 6;
FIG. 8 is an exploded view of the internal structure of FIG. 4;
FIG. 9 is a cross-sectional view showing the internal structure of the fabrication tower and the sub-drum of FIG. 1;
FIG. 10 is a schematic diagram showing the upper structure of the servo motor and the reaction plate in FIG. 9;
FIG. 11 is an enlarged view of the connection between the drive roller and the two linked rollers of FIG. 10;
FIG. 12 is an enlarged view of the connection structure between the reaction plate and the two interlocking rollers in FIG. 10;
Fig. 13 is an upper schematic view of the air feed pump of fig. 9.
In the figure: the device comprises a preparation tower 1, a formaldehyde inlet pipe 2, a sulfuric acid inlet pipe 3, an accessory barrel 4, a phosphine inlet pipe 5, a collecting pipe 6, a collecting arc disk 7, a spraying box 8, a servo motor 9, a bearing disk 10, a reaction disk 11, a fixing frame 12, a driving roller 13, a driven roller 14, a stirring rod 15, a scooping spoon 16, a liquid discharging pipe 17, an electric self-locking wheel I18, a self-reset rotary roller 19, a squeezing disk 20, a reciprocating screw rod 21, a spraying hole 22, a ball nut 23, a gas feeding pump 24, a gas feeding pipe 25, a 26 arc-shaped groove 26, a driven bevel gear 27, a driving bevel gear 28, a 29 temperature control heating plate 30, an electric self-locking wheel III, a 31 linkage roller 32, a fixing wheel 33, a liquid containing groove 34, a liquid passing pipe 35, a gas spraying pipe 36, a gas spraying diffusion cover 37 and a stirring hole.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
Referring to fig. 1 to 3, a preparation device of the tetrakis (hydroxymethyl) phosphonium sulfate comprises a preparation tower 1, wherein the preparation tower 1 is used for performing efficient preparation work of the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution;
Referring to fig. 1 to 6, the mixing and stirring part is used for sufficiently and uniformly mixing the formaldehyde solution and the sulfuric acid solution, so that the preparation efficiency of the aqueous solution of the tetrakis (hydroxymethyl) phosphonium sulfate is improved;
The mixing and stirring part comprises a formaldehyde inlet pipe 2 for feeding formaldehyde solution, which is fixedly arranged on the preparation tower 1, a sulfuric acid inlet pipe 3 for feeding sulfuric acid solution is fixedly arranged on the preparation tower 1, a servo motor 9 is fixedly arranged at the bottom of the preparation tower 1, and a driving roller 13 is fixedly arranged on the driving end of the servo motor 9;
The preparation tower 1 is internally and fixedly provided with a collecting arc disk 7 for bearing formaldehyde solution and sulfuric acid solution, when the preparation of the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution is carried out, the formaldehyde solution and the sulfuric acid solution are respectively injected into the preparation tower 1 through a formaldehyde inlet pipe 2 and a sulfuric acid inlet pipe 3 according to the mol ratio of 8:1, so that the formaldehyde solution and the sulfuric acid solution are accumulated on the collecting arc disk 7 in the preparation tower 1 and are preliminarily mixed;
The driving roller 13 is provided with a stirring mechanism, the stirring mechanism comprises a driven roller 14 fixedly arranged on the driving roller 13, the driven roller 14 is matched with an electric self-locking wheel I18, a plurality of fixing frames 12 are fixedly arranged on the electric self-locking wheel I18, each fixing frame 12 is rotatably provided with a self-resetting rotating roller 19, each self-resetting rotating roller 19 is fixedly provided with a plurality of stirring rods 15, and each stirring rod 15 is provided with a plurality of stirring holes 37;
After the primary fusion is finished, a servo motor 9 is started to drive a driving roller 13 and a driven roller 14 to rotate, an electric self-locking wheel I18 is started to jointly rotate the driving roller 13 and the driven roller 14, the electric self-locking wheel I18 rotates to drive stirring rods 15 in a plurality of stirring mechanisms to synchronously rotate, and formaldehyde solution and sulfuric acid solution can be sufficiently stirred to be uniformly mixed;
The self-resetting rotary roller 19 is a spring rod body which is commonly used in the prior art and can automatically reset after rotating, and is not repeated here;
The stirring rod 15 rotates and stirs, and can generate reciprocating swing under the cooperation rotation of the self-resetting rotating roller 19, so that the contact range and the contact area between the stirring rod 15 and the formaldehyde solution and the sulfuric acid solution can be further increased, the stirring and mixing efficiency of the formaldehyde solution and the sulfuric acid solution can be further increased, and the formaldehyde solution and the sulfuric acid solution can be mixed more uniformly.
Referring to fig. 4, 6-8, the solution spraying part is used for enabling the formaldehyde and sulfuric acid mixed solution to be sprayed downwards quickly and uniformly, so that the formaldehyde and sulfuric acid mixed solution can be in contact reaction with phosphine gas more uniformly and fully;
The solution spraying part comprises a spraying box 8 fixedly arranged at the lower part of the collecting arc disc 7, a liquid discharging structure is arranged between the collecting arc disc 7 and the spraying box 8, the liquid discharging structure comprises a plurality of liquid discharging pipes 17 fixedly communicated between the spraying box 8 and the collecting arc disc 7, after the formaldehyde solution and the sulfuric acid solution are stirred and mixed, the liquid discharging pipes 17 can be opened to enable the mixed solution to enter the lower part of the extrusion plate 20 in the spraying box 8 through the liquid discharging pipes 17 and be accumulated, and the transfer of the formaldehyde solution and the sulfuric acid solution is completed;
an extrusion mechanism is arranged between the driving roller 13 and the spraying box 8, the extrusion mechanism comprises an extrusion disc 20 which is arranged in the spraying box 8 through a sliding limiting structure, an electric self-locking wheel II is arranged on the driven roller 14 in a matched mode, a reciprocating screw rod 21 is fixedly arranged on the electric self-locking wheel II, a ball nut 23 is arranged on the reciprocating screw rod 21 in a matched mode, and the ball nut 23 is fixedly connected with the extrusion disc 20;
After formaldehyde and sulfuric acid mixed solution enters the spray box 8, the electric self-locking wheel II can be started to be locked with the driven roller 14, and then the servo motor 9 is started to drive the driving roller 13, the driven roller 14 and the electric self-locking wheel II to rotate, so that the reciprocating screw rod 21 is driven to rotate, and the extrusion disc 20 can be driven to reciprocate up and down under the cooperation of the ball nut 23;
The sliding limiting structure comprises a plurality of limiting sliding rods fixedly arranged on the extrusion disc 20, a plurality of limiting sliding grooves are formed in the inner wall of the spraying box 8, the limiting sliding rods are respectively clamped and slidably arranged in the corresponding limiting sliding grooves, and two limiting spring rods are fixedly arranged between the extrusion disc 20 and the inner wall of the spraying box 8;
The limiting sliding structure is used for enabling the extrusion disc 20 to vertically slide in a limiting manner only in the spraying box 8 without being deviated and separated from the spraying box 8;
The plurality of liquid discharging pipes 17 are in sliding connection with the extrusion disc 20, the lower part of the spray box 8 is provided with a plurality of spray holes 22, the inner wall of each spray hole 22 is fixedly provided with an elastic taper ring, the extrusion disc 20 can extrude the mixed solution at the lower part of the extrusion disc in a reciprocating manner when descending, and the mixed solution is sprayed into the preparation tower 1 in a reciprocating intermittent manner after passing through the elastic taper rings in the spray holes 22, so that the dispersion range of formaldehyde and sulfuric acid mixed solution is improved, and the reaction efficiency is improved;
The whole shape of the elastic conical ring is set as an inverted cone, the lower part of the elastic conical ring is provided with a communicating hole for passing liquid, the elastic conical ring is integrally made of rubber elastic materials, when the elastic conical ring is subjected to the pressure of liquid, the communicating hole at the lower part of the elastic conical ring can be increased under the pressure of the liquid, at the moment, formaldehyde and sulfuric acid mixed solution can pass through the communicating hole downwards to pass through the liquid, when the mixed solution is not subjected to the pressure of the liquid, the aperture of the communicating hole is smaller, and large-flow liquid passing can not be carried out, so that the liquid passing speed is controlled, and intermittent spraying and discharging are realized.
Referring to fig. 2, 9-13, the absorption reaction part is used for carrying out rapid reaction of phosphine gas and formaldehyde and sulfuric acid mixed solution, so as to efficiently prepare the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution;
The specific reaction equation of the formaldehyde, sulfuric acid mixed solution and phosphine gas is as follows:
8HCHO+H2SO4+2PH3＝[(CH2OH)4P]2SO4；
The absorption reaction part comprises two linkage rollers 31 rotatably arranged on the preparation tower 1, an air inlet mechanism for the phosphine gas is arranged on the preparation tower 1, the air inlet mechanism comprises an auxiliary barrel 4 fixedly arranged on the preparation tower 1, a phosphine inlet pipe 5 for feeding the phosphine gas is fixedly arranged in the auxiliary barrel 4, an upper air pipe 25 is fixedly arranged on the air outlet end of the air supply pump 24, and a plurality of air injection pipes 35 are fixedly arranged between the upper air pipe 25 and the preparation tower 1;
While spraying the formaldehyde and sulfuric acid mixed solution, the air supply pump 24 starts to spray phosphine gas in the accessory barrel 4 into the preparation tower 1 through the upper air pipe 25 and the plurality of air injection pipes 35, and fully contacts and reacts with the formaldehyde and sulfuric acid mixed solution, and the temperature in the preparation tower 1 is controlled between 50-60 ℃, so that the preparation work of the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution can be started;
Each air jet pipe 35 is fixedly provided with an air jet diffusion cover 36, and the air jet diffusion cover 36 is used for further increasing the spraying range of phosphine gas, so that the reaction preparation efficiency is improved;
A linkage mechanism is arranged between the two linkage rollers 31 and the driving roller 13, the linkage mechanism comprises an electric self-locking wheel III 30 fixedly arranged on the driving roller 13, a driving bevel gear 28 is fixedly arranged on the electric self-locking wheel III 30, driven bevel gears 27 are fixedly arranged on the two linkage rollers 31, and the two driven bevel gears 27 are meshed with the driving bevel gears 28;
when the reaction is carried out, the electric self-locking wheel III 30 is started to be locked with the driving roller 13, and the servo motor 9 is started to drive the driving roller 13 to rotate, the electric self-locking wheel III 30 is driven to rotate, namely the driving bevel gear 28 is driven to rotate, so that the two linkage rollers 31 are driven to rotate together under the cooperation of the two driven bevel gears 27;
The electric self-locking wheel I18, the electric self-locking wheel II and the electric self-locking wheel III 30 are common accessories which can realize self-locking with an external rod body after starting in the prior art, and specific operation modes can refer to self-locking universal wheels adopted in the application number CN202022504746.X and are not described in detail herein;
The two linkage rollers 31 are provided with a scooping mechanism, the scooping mechanism comprises a fixed wheel 32 fixedly arranged on the linkage rollers 31, a plurality of scooping spoons 16 are fixedly arranged on the fixed wheel 32, each scooping spoon 16 is provided with a liquid containing groove 33, a reaction disc 11 is fixedly arranged in the preparation tower 1, the reaction disc 11 is provided with an arc-shaped groove 26 matched with the plurality of scooping spoons 16, and the arc-shaped groove 26 is used for bearing a tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution;
The two linkage rollers 31 rotate to drive the plurality of scooping and dispersing scoops 16 to rotate under the cooperation of the fixed wheels 32, and when the scooping and dispersing scoops 16 rotate, the formaldehyde and sulfuric acid mixed solution in the arc-shaped groove 26 is scooped up and fully diffused in the preparation tower 1 under the cooperation of the liquid containing groove 33, so that the formaldehyde and sulfuric acid mixed solution can be fully contacted and reacted with phosphine gas, and the reaction efficiency is improved;
the back side of each scooping and scattering scoop 16 is fixedly provided with a temperature control heating plate 29 for heating, the formaldehyde, sulfuric acid mixed solution and phosphine gas can be heated when the temperature control heating plates 29 are synchronously started, and the temperature in the preparation tower 1 is regulated and controlled, so that the temperature in the preparation tower 1 is always kept between 50-60 ℃, and the formaldehyde, sulfuric acid mixed solution and phosphine gas always react in a constant temperature environment, and the reaction efficiency is higher;
A collecting mechanism is arranged in the preparation tower 1 and comprises a bearing disc 10 fixedly arranged on the preparation tower 1, a plurality of liquid passing pipes 34 are fixedly arranged on the reaction disc 11, liquid outlet ends of the liquid passing pipes 34 are positioned at the lower part of the bearing disc 10, and a collecting pipe 6 matched with the bearing disc 10 is fixedly arranged on the preparation tower 1;
After the formaldehyde and sulfuric acid mixed solution reacts with phosphine gas, a tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution is generated and is accumulated in the arc-shaped groove 26 on the reaction disc 11, a plurality of liquid passing pipes 34 can be opened to enable the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution to fall into the bearing disc 10, and a collecting pipe 6 is opened to take out and collect the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution;
the control valves are arranged on the liquid passing pipes 34, the air spraying pipes 35, the phosphine inlet pipe 5, the liquid discharging pipes 17, the formaldehyde inlet pipe 2 and the sulfuric acid inlet pipe 3, and the opening and closing states of the pipes can be controlled through the control valves, so that the preparation of the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution is more orderly and efficient.
A preparation process of a preparation device of tetrakis (hydroxymethyl) phosphonium sulfate comprises the following steps:
S1, when the preparation of the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution is carried out, firstly, formaldehyde solution and sulfuric acid solution are respectively injected into a preparation tower 1 through a formaldehyde inlet pipe 2 and a sulfuric acid inlet pipe 3 according to the mol ratio of 8:1, so that the formaldehyde solution and the sulfuric acid solution are accumulated on a collecting arc disk 7 in the preparation tower 1;
S2, restarting the servo motor 9 to drive the driving roller 13 and the driven roller 14 to rotate, starting the electric self-locking wheel I18 to jointly rotate the driving roller 13 and the driven roller 14, and enabling the electric self-locking wheel I18 to rotate so as to drive stirring rods 15 in a plurality of stirring mechanisms to synchronously rotate, so that formaldehyde solution and sulfuric acid solution can be sufficiently stirred to be uniformly mixed;
s3, after the formaldehyde solution and the sulfuric acid solution are stirred and mixed, a plurality of liquid discharging pipes 17 can be opened to enable the mixed solution to enter the lower portion of an extrusion disc 20 in the spray box 8 through the liquid discharging pipes 17 and be accumulated, and transfer of the formaldehyde solution and the sulfuric acid solution is completed;
s4, restarting the electric self-locking wheel II to lock with the driven roller 14, starting the servo motor 9 to drive the driving roller 13, the driven roller 14 and the electric self-locking wheel II to rotate, so as to drive the reciprocating screw rod 21 to rotate, namely, driving the extrusion disc 20 to reciprocate up and down under the cooperation of the ball nut 23, and extruding the mixed solution at the lower part of the extrusion disc 20 in a reciprocating manner when the extrusion disc 20 descends, so that the mixed solution is sprayed into the preparation tower 1 in a reciprocating intermittent manner through the plurality of spraying holes 22;
S5, spraying the mixed solution of formaldehyde and sulfuric acid, and simultaneously starting an air supply pump 24 to spray phosphine gas in an accessory barrel 4 into the preparation tower 1 through an upper air pipe 25 and a plurality of air injection pipes 35, and fully contacting and reacting with the mixed solution of formaldehyde and sulfuric acid, wherein a plurality of temperature control heating plates 29 synchronously start heating the mixed solution of formaldehyde and sulfuric acid, and the temperature in the preparation tower 1 is controlled between 50-60 ℃, so that the preparation work of the aqueous solution of the tetrakis (hydroxymethyl) phosphonium sulfate can be started;
S6, when the reaction is carried out, the electric self-locking wheel III 30 is started to be locked with the driving roller 13, and when the servo motor 9 is started to drive the driving roller 13 to rotate, the electric self-locking wheel III 30 is driven to rotate, namely the driving bevel gear 28 is driven to rotate, so that the two linkage rollers 31 are driven to rotate together under the cooperation of the two driven bevel gears 27;
S7, the two linkage rollers 31 rotate to drive the plurality of scooping spoons 16 to rotate under the cooperation of the fixed wheels 32, and when the scooping spoons 16 rotate, the mixed solution of formaldehyde and sulfuric acid in the arc-shaped groove 26 is scooped up to be fully diffused in the preparation tower 1, so that the mixed solution of formaldehyde and sulfuric acid can be fully contacted and reacted with phosphine gas, and the reaction efficiency is improved;
And S8, after the mixed solution of formaldehyde and sulfuric acid is reacted with phosphine gas, generating a tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution, accumulating the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution in an arc-shaped groove 26 on the reaction tray 11, opening a plurality of liquid passing pipes 34 to enable the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution to fall into the bearing tray 10, and opening a collecting pipe 6 to take out and collect the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (7)
1. The preparation device of the tetrakis (hydroxymethyl) phosphonium sulfate is characterized by comprising a preparation tower (1);
The mixing and stirring part comprises a formaldehyde inlet pipe (2) for feeding formaldehyde solution, which is fixedly arranged on a preparation tower (1), wherein a sulfuric acid inlet pipe (3) for feeding sulfuric acid solution is fixedly arranged on the preparation tower (1), a servo motor (9) is fixedly arranged at the bottom of the preparation tower (1), a driving roller (13) is fixedly arranged on the driving end of the servo motor (9), a stirring mechanism is arranged on the driving roller (13), the stirring mechanism comprises a driven roller (14) fixedly arranged on the driving roller (13), an electric self-locking wheel I (18) is matched and arranged on the driven roller (14), a plurality of fixing frames (12) are fixedly arranged on the electric self-locking wheel I (18), a self-resetting rotary roller (19) is rotatably arranged on each fixing frame (12), a plurality of stirring rods (15) are fixedly arranged on each self-resetting rotary roller (19), and a collecting arc disc (7) for bearing formaldehyde solution and sulfuric acid solution is fixedly arranged in the preparation tower (1);
The solution spraying part is used for enabling formaldehyde and sulfuric acid mixed solution to spray downwards rapidly and uniformly, the solution spraying part comprises a spraying box (8) fixedly arranged at the lower part of a collecting arc disc (7), an extrusion mechanism is arranged between a driving roller (13) and the spraying box (8), the extrusion mechanism comprises an extrusion disc (20) arranged in the spraying box (8) through a sliding limiting structure, an electric self-locking wheel II is arranged on a driven roller (14) in a matched manner, a reciprocating screw rod (21) is fixedly arranged on the electric self-locking wheel II, a ball nut (23) is arranged on the reciprocating screw rod (21) in a matched manner, the ball nut (23) is fixedly connected with the extrusion disc (20), and a liquid discharging structure is arranged between the collecting arc disc (7) and the spraying box (8);
The liquid discharging structure comprises a plurality of liquid discharging pipes (17) fixedly communicated between the spraying box (8) and the collecting arc disc (7), and a plurality of spraying holes (22) are formed in the lower portion of the spraying box (8);
The absorption reaction part is used for carrying out rapid reaction of phosphine gas, formaldehyde and sulfuric acid mixed solution to prepare a tetrakis hydroxymethyl phosphonium sulfate aqueous solution, the absorption reaction part comprises two linkage rollers (31) rotatably arranged on a preparation tower (1), a linkage mechanism is arranged between the two linkage rollers (31) and a driving roller (13), the linkage mechanism comprises an electric self-locking wheel III (30) fixedly arranged on the driving roller (13), a driving bevel gear (28) is fixedly arranged on the electric self-locking wheel III (30), driven bevel gears (27) are fixedly arranged on the two linkage rollers (31), and the two driven bevel gears (27) are meshed with the driving bevel gears (28);
The two linkage rollers (31) are provided with a scooping mechanism, the scooping mechanism comprises a fixed wheel (32) fixedly arranged on the linkage rollers (31), a plurality of scooping spoons (16) are fixedly arranged on the fixed wheel (32), and a temperature control heating plate (29) for heating is fixedly arranged on the back side of each scooping spoon (16);
A reaction disc (11) is fixedly installed in the preparation tower (1), an arc-shaped groove (26) matched with a plurality of scooping and scattering spoons (16) is formed in the reaction disc (11), the arc-shaped groove (26) is used for bearing a tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution, an air inlet mechanism for the air inlet of phosphine gas is installed on the preparation tower (1), the air inlet mechanism comprises an accessory barrel (4) fixedly installed on the preparation tower (1), an upper air pipe (25) is fixedly installed at the air outlet end of an air supply pump (24), a plurality of air injection pipes (35) are fixedly installed between the upper air pipe (25) and the preparation tower (1), a collecting mechanism is installed in the preparation tower (1), the collecting mechanism comprises a bearing disc (10) fixedly installed on the preparation tower (1), a plurality of liquid passing pipes (34) are fixedly installed on the reaction disc (11), and a collecting pipe (6) matched with the bearing disc (10) is fixedly installed on the preparation tower (1);
the preparation process applied to the preparation device comprises the following steps:
S1, when the preparation of the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution is carried out, firstly, formaldehyde solution and sulfuric acid solution are respectively injected into a preparation tower (1) through a formaldehyde inlet pipe (2) and a sulfuric acid inlet pipe (3) according to the mol ratio of 8:1, so that the formaldehyde solution and the sulfuric acid solution are accumulated on a collecting arc disc (7) in the preparation tower (1);
S2, restarting the servo motor (9) to drive the driving roller (13) and the driven roller (14) to rotate, starting the electric self-locking wheel I (18) to jointly rotate the driving roller (13) and the driven roller (14), and enabling the electric self-locking wheel I (18) to rotate so as to drive stirring rods (15) in a plurality of stirring mechanisms to synchronously rotate, so that formaldehyde solution and sulfuric acid solution can be sufficiently stirred to be uniformly mixed;
s3, after the formaldehyde solution and the sulfuric acid solution are stirred and mixed, a plurality of liquid discharging pipes (17) can be opened to enable the mixed solution to enter the lower part of an extrusion disc (20) in the spraying box (8) through the liquid discharging pipes (17) and be accumulated, and transfer of the formaldehyde solution and the sulfuric acid solution is completed;
S4, restarting the electric self-locking wheel II to lock the driven roller (14), and starting the servo motor (9) to drive the driving roller (13), the driven roller (14) and the electric self-locking wheel II to rotate so as to drive the reciprocating screw rod (21) to rotate, namely, driving the extrusion disc (20) to reciprocate up and down under the cooperation of the ball nut (23), and repeatedly extruding the mixed solution at the lower part of the extrusion disc (20) when the extrusion disc descends, so that the mixed solution is intermittently sprayed into the preparation tower (1) in a reciprocating manner through the plurality of spraying holes (22);
S5, spraying the mixed solution of formaldehyde and sulfuric acid, and simultaneously starting an air supply pump (24) to spray phosphine gas in an auxiliary barrel (4) into the preparation tower (1) through an upper air pipe (25) and a plurality of air injection pipes (35), and fully contacting and reacting the mixed solution of formaldehyde and sulfuric acid, wherein a plurality of temperature control heating plates (29) synchronously start heating the mixed solution of formaldehyde and sulfuric acid, and the temperature in the preparation tower (1) is controlled between 50-60 ℃, so that the preparation of the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution can be started;
s6, when the reaction is carried out, the electric self-locking wheel III (30) is started to be locked with the driving roller (13), and when the servo motor (9) is started to drive the driving roller (13) to rotate, the electric self-locking wheel III (30) is driven to rotate, namely the driving bevel gear (28) is driven to rotate, so that the two linkage rollers (31) are driven to rotate together under the cooperation of the two driven bevel gears (27);
S7, the two linkage rollers (31) rotate to drive the plurality of scooping and dispersing scoops (16) to rotate under the cooperation of the fixed wheels (32), and when the scooping and dispersing scoops (16) rotate, the mixed solution of formaldehyde and sulfuric acid in the arc-shaped groove (26) is scooped up to be fully diffused in the preparation tower (1), so that the mixed solution of formaldehyde and sulfuric acid can be fully contacted and reacted with phosphine gas, and the reaction efficiency is improved;
S8, after the mixed solution of formaldehyde and sulfuric acid is reacted with phosphine gas, generating a tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution, stacking the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution in an arc-shaped groove (26) on a reaction disc (11), opening a plurality of liquid passing pipes (34) to enable the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution to fall into a bearing disc (10), and opening a collecting pipe (6) to take out and collect the tetrakis (hydroxymethyl) phosphonium sulfate aqueous solution.
2. The preparation device of the tetrakis (hydroxymethyl) phosphonium sulfate according to claim 1, wherein a plurality of stirring holes (37) are formed in each stirring rod (15).
3. The preparation device of the tetrakis (hydroxymethyl) phosphonium sulfate according to claim 1, wherein a plurality of the downcomers (17) are in sliding connection with the extrusion disc (20), and an elastic conical ring is fixedly arranged on the inner wall of each spraying hole (22).
4. The preparation device of the tetrakis hydroxymethyl phosphonium sulfate according to claim 1, wherein the sliding limiting structure comprises a plurality of limiting sliding rods fixedly installed on the extrusion disc (20), a plurality of limiting sliding grooves are formed in the inner wall of the spraying box (8), the limiting sliding rods are respectively clamped and slidably installed in the corresponding limiting sliding grooves, and two limiting spring rods are fixedly installed between the extrusion disc (20) and the inner wall of the spraying box (8).
5. The preparation device of the tetrakis (hydroxymethyl) phosphonium sulfate according to claim 1, wherein each scooping scoop (16) is provided with a liquid containing tank (33), and a phosphine inlet pipe (5) for feeding phosphine gas is fixedly arranged in the auxiliary barrel (4).
6. The preparation device of the tetrakis (hydroxymethyl) phosphonium sulfate according to claim 1, wherein each gas jet pipe (35) is fixedly provided with a gas jet diffusion cover (36).
7. The preparation device of the tetrakis (hydroxymethyl) phosphonium sulfate according to claim 1, wherein the liquid outlet ends of the plurality of liquid passing pipes (34) are all positioned at the lower part of the bearing disc (10), and the plurality of liquid passing pipes (34), the plurality of air injection pipes (35), the phosphine inlet pipe (5), the plurality of liquid discharging pipes (17), the formaldehyde inlet pipe (2) and the sulfuric acid inlet pipe (3) are all provided with control valves.
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| CN202410155666.8A CN117680083B (en) | 2024-02-04 | 2024-02-04 | Preparation process and preparation device of tetrakis (hydroxymethyl) phosphonium sulfate |
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| CN202410155666.8A CN117680083B (en) | 2024-02-04 | 2024-02-04 | Preparation process and preparation device of tetrakis (hydroxymethyl) phosphonium sulfate |
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| CN117680083A (en) | 2024-03-12 |
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