CN110665448A - Phosphite ester preparation method and phosphite ester reaction kettle - Google Patents
Phosphite ester preparation method and phosphite ester reaction kettle Download PDFInfo
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- CN110665448A CN110665448A CN201911128616.6A CN201911128616A CN110665448A CN 110665448 A CN110665448 A CN 110665448A CN 201911128616 A CN201911128616 A CN 201911128616A CN 110665448 A CN110665448 A CN 110665448A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 63
- 150000008301 phosphite esters Chemical class 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 328
- 238000001816 cooling Methods 0.000 claims abstract description 64
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000004804 winding Methods 0.000 claims abstract description 9
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 11
- 238000001514 detection method Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 230000000149 penetrating effect Effects 0.000 claims description 4
- 239000000110 cooling liquid Substances 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 4
- 239000002826 coolant Substances 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- 230000007774 longterm Effects 0.000 abstract description 2
- 230000008602 contraction Effects 0.000 description 8
- 239000003963 antioxidant agent Substances 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
Classifications
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- 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
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/05—Stirrers
- B01F27/051—Stirrers characterised by their elements, materials or mechanical properties
- B01F27/054—Deformable stirrers, e.g. deformed by a centrifugal force applied during operation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/05—Stirrers
- B01F27/11—Stirrers characterised by the configuration of the stirrers
- B01F27/19—Stirrers with two or more mixing elements mounted in sequence on the same axis
- B01F27/191—Stirrers with two or more mixing elements mounted in sequence on the same axis with similar elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/141—Esters of phosphorous acids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F2035/98—Cooling
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00092—Tubes
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention relates to a phosphite ester preparation method and a phosphite ester reaction kettle, which comprise a reaction tank body (1) and a supporting tank body (2), wherein the reaction tank body (1) is supported and arranged above the supporting tank body (2), the distance between each stirring blade and a stirring shaft can be adjusted in real time according to the height position of a mixture in the reaction kettle, and the mixture can be uniformly and fully stirred with the most suitable stirring radius, so that the uniform mixing and full reaction in the reaction kettle are ensured; set up tank shell body to including shell body and interior casing simultaneously, and spiral winding has outer cooling coil on the outer wall of shell body, and spiral winding has interior cooling coil on the outer wall of shell body to realize the whole cooling effect to tank shell body internal mixing environment through inside and outside double-deck cooling coil, because inside and outside double-deck cooling coil's setting exposes outside cooling temperature can not obtain the defect of long-term stable assurance and then need frequently changing the coolant liquid in the course of the work.
Description
Technical Field
The invention relates to the technical field of phosphite ester preparation, and particularly relates to a phosphite ester preparation method and a phosphorous acid reaction kettle.
Background
In recent years, the demand for global antioxidant markets has increased rapidly. Due to the steady development of the global market, the demand of phosphite antioxidants is kept in a relatively stable state in future. In the prior art, most production processes related to phosphite antioxidants are monopolized abroad, and the production processes adopted by domestic manufacturers still have the problems of more operation steps, complex operation, low yield of a single kettle, high unit consumption, incapability of continuous operation of production and the like.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the invention aims to provide a phosphite ester preparation method and a phosphite ester reaction kettle.
The technical scheme adopted by the invention is as follows:
a phosphite ester preparation method, which is characterized in that: the method comprises the following steps:
1) feeding a first raw material and a second raw material into the reaction tank body through a first feeding port and a second feeding port respectively;
2) after a catalyst is fed into the reaction tank body through the stirring shaft inlet, the stirring shaft is connected with a driving source through a master controller, signal connection between the first stirring controller and the first stirring assembly, between the second stirring controller and the second stirring assembly and between the third stirring controller and the third stirring assembly is confirmed to be smooth, and corresponding height positions H1, H2 and H3 of the first stirring assembly, the second stirring assembly and the third stirring assembly are recorded through the master controller respectively;
3) respectively winding an inner cooling coil on the outer wall of the inner shell through an inlet of the inner coil and then penetrating out through an outlet of the inner coil, winding an outer cooling coil on the outer wall of the outer shell through an inlet of the outer coil and then penetrating out through an outlet of the outer coil, and respectively injecting cooling liquid into the outer cooling coil and the inner cooling coil;
4) starting a driving source to drive a stirring shaft to respectively drive a first stirring assembly, a second stirring assembly and a third stirring assembly to synchronously rotate; a material thickness detection device arranged on the inner wall of the inner shell detects the axial thickness real-time value H0 of the mixture inside the inner shell in real time;
when and only when H0 is more than or equal to H1, the master controller adjusts the rotating speed of the stirring shaft to be increased from R0 to R1, meanwhile, the first stirring controller controls the first stirring blade to increase the distance relative to the stirring shaft through the first telescopic device, the second stirring controller controls the second stirring blade to increase the distance relative to the stirring shaft through the second telescopic device, and the third stirring controller controls the third stirring blade to increase the distance relative to the stirring shaft through the third telescopic device;
when H1 is more than H0 and is more than or equal to H2, the master controller adjusts the rotating speed of the stirring shaft to be increased from R0 to R2, meanwhile, the first stirring controller controls the distance between the first stirring blades and the stirring shaft to be unchanged, the second stirring controller controls the distance between the second stirring blades and the stirring shaft to be increased through the second expansion device, and the third stirring controller controls the distance between the third stirring blades and the stirring shaft to be increased through the third expansion device;
when H2 is more than H0 and is more than or equal to H3, the master controller adjusts the rotating speed of the stirring shaft to be increased from R0 to R3, meanwhile, the first stirring controller controls the distance between the first stirring blades and the stirring shaft to be constant, the second stirring controller controls the distance between the second stirring blades and the stirring shaft to be constant, and the third stirring controller controls the third stirring blades to increase the distance between the third stirring blades and the stirring shaft through a third telescopic device;
when and only when H3 is more than H0, the master controller keeps the rotation speed of the stirring shaft to be gradually reduced, and simultaneously controls the distance between the first stirring blade and the stirring shaft to be constant through the first stirring controller, controls the distance between the second stirring blade and the stirring shaft to be constant through the second stirring controller, and controls the distance between the third stirring blade and the stirring shaft to be constant through the third stirring controller;
and R1 > R2 > R3 > R0;
5) keeping the corresponding reaction process for 1-2h at the temperature of 45-60 ℃, and discharging the obtained product from a lower discharge port after filtering;
6) and carrying out flash evaporation in the reaction tank body, and discharging the obtained gas product through an upper vent.
Further, the present invention provides a phosphite ester reaction kettle used in the above-mentioned phosphite ester production method, characterized in that: the device comprises a reaction tank body and a supporting tank body, wherein the reaction tank body is supported and arranged above the supporting tank body; wherein,
the reaction tank body comprises a tank body top cover positioned at the top, a tank body shell positioned at the middle and a tank body bottom support positioned at the bottom, the tank body shell comprises an outer shell and an inner shell, an outer cooling coil is spirally wound on the outer wall of the outer shell, an inner cooling coil is spirally wound on the outer wall of the inner shell, an outer coil inlet is arranged above one side of the outer shell, an inner coil inlet, an inner coil outlet and an outer coil outlet are sequentially arranged on the other side of the outer shell from top to bottom, and a material thickness detection device is arranged on the inner wall of the inner shell;
a first feeding port, a second feeding port and a stirring shaft inlet are respectively formed above the tank body top cover, the first feeding port and the second feeding port are respectively arranged on two sides of the stirring shaft inlet, a standby port and a sampling port are also formed in one side, close to the first feeding port, above the tank body top cover, a vent is further formed in one side, close to the second feeding port, above the tank body top cover, a temperature detection device is further inserted into the tank body shell in a direction obliquely downward to the tank body bottom support, an observation window is further formed in the outer wall of the supporting tank body, and a discharge port extends out of the lower end of the tank body bottom support and transversely penetrates out of the outer wall of the supporting tank body;
the stirring shaft extends into the reaction tank body from the inlet of the stirring shaft, the stirring shaft is arranged in the reaction tank body, the stirring shaft is driven by an external driving source to rotate, the rotation speed control is realized through a master controller, and a first stirring assembly, a second stirring assembly and a third stirring assembly are sequentially arranged on the stirring shaft from top to bottom, wherein the first stirring assembly comprises a first stirring blade which is connected with the stirring shaft through a first telescopic device and can realize the distance adjustment of the first stirring blade relative to the stirring shaft under the control of the first stirring controller; the second stirring assembly comprises a second stirring blade, the second stirring blade is connected with the stirring shaft through a second telescopic device and can realize the distance adjustment of the second stirring blade relative to the stirring shaft under the control of a second stirring controller; the third stirring subassembly includes third stirring vane, third stirring vane via the third telescoping device with stirring shaft connection just can realize realizing under the control of third stirring controller third stirring vane for the interval control of (mixing) shaft, first stirring controller, second stirring controller and third stirring controller respectively with total controller signal connection.
Further, the outer cooling coil is spirally wound on the outer wall below the bottom support of the tank body.
Further, the pitch of the outer cooling coil of two adjacent circles is larger than that of the inner cooling coil of two adjacent circles.
Further, the pipe diameter of the outer cooling coil is smaller than that of the inner cooling coil.
Further, the axial positions of the first stirring assembly, the second stirring assembly and the third stirring assembly on the stirring shaft can be adjusted.
Further, a filter screen assembly is arranged between the tank body shell and the tank body bottom support.
Further, the first stirring blade, the second stirring blade and the third stirring blade are the same in size.
Furthermore, the telescopic stroke of the first telescopic device is slightly smaller than that of the second telescopic device, and the telescopic stroke of the second telescopic device is slightly smaller than that of the third telescopic device.
Further, a loading and unloading flange is arranged on the stirring shaft above the first stirring assembly.
Compared with the prior art, the invention has the following technical effects:
(1) can adjust in real time each stirring vane for the interval of (mixing) shaft according to the mixture in the inside high position of reation kettle in real time, can realize the even and intensive mixing to the mixture with the most suitable stirring radius to guarantee that the inside misce bene of reation kettle reacts fully.
(2) Set up tank shell body to including shell body and interior casing simultaneously, and spiral winding has outer cooling coil on the outer wall of shell body, and spiral winding has interior cooling coil on the outer wall of shell body to realize the whole cooling effect to tank shell body internal mixing environment through inside and outside double-deck cooling coil, because inside and outside double-deck cooling coil's setting exposes outside cooling temperature can not obtain the defect of long-term stable assurance and then need frequently changing the coolant liquid in the course of the work.
Drawings
FIG. 1 is a schematic diagram of the structure of a phosphite reaction kettle of the present invention.
Detailed Description
As shown in fig. 1, a phosphite ester reaction kettle comprises a reaction tank body 1 and a supporting tank body 2, wherein the reaction tank body 1 is supported and arranged above the supporting tank body 2; wherein,
the reaction tank body 1 comprises a tank body top cover 1-1 positioned at the top of the upper part, a tank body shell 1-2 positioned at the middle part and a tank body bottom support 1-3 positioned at the bottom, the tank body shell 1-2 comprises an outer shell 1-21 and an inner shell 1-22, an outer cooling coil 1-2a is spirally wound on the outer wall of the outer shell 1-21, an inner cooling coil 1-2b is spirally wound on the outer wall of the inner shell 1-22, an outer coil inlet a-1 is arranged above one side of the outer shell 1-21, an inner coil inlet b-1, an inner coil outlet b-2 and an outer coil outlet a-2 are sequentially arranged on the other side of the outer shell 1-21 from top to bottom, and a material thickness detection device is arranged on the inner wall of the inner shell 1-22;
a first feeding port 3, a second feeding port 4 and a stirring shaft inlet port 5 are respectively arranged above a tank top cover 1-1, the first feeding port 3 and the second feeding port 4 are respectively arranged at two sides of the stirring shaft inlet port 5, a standby port 6 (used as a standby feeding port) and a sampling port 7 (used for sampling for testing when the reaction is carried out to a specific stage) are also arranged at one side above the tank top cover 1-1 and close to the first feeding port 3, a vent 8 (used for communicating with outside air) is also arranged at one side above the tank top cover 1-1 and close to the second feeding port 4, a temperature detection device 9 is inserted and arranged in the direction of a tank body bottom support 1-3 obliquely below a tank body shell 1-2 for detecting the temperature change in the reaction process in real time, an observation window 10 is also arranged on the outer wall of a supporting tank body 2, a discharge port 11 is extended from the lower end of the tank bottom support 1-3 and transversely penetrates out of (ii) a
A stirring shaft 13 is arranged in the reaction tank body 1 extending from a stirring shaft inlet 5, the stirring shaft 13 is driven by an external driving source M to rotate and realize rotation speed control through a master controller C, a first stirring assembly 13-1, a second stirring assembly 13-2 and a third stirring assembly 13-3 are sequentially arranged on the stirring shaft 13 from top to bottom, wherein the first stirring assembly 13-1 comprises a first stirring blade 13-12, the first stirring blade 13-12 is connected with the stirring shaft 13 through a first telescopic device 13-11 and can realize the distance adjustment of the first stirring blade 13-12 relative to the stirring shaft 13 under the control of the first stirring controller C1; the second stirring assembly 13-2 comprises a second stirring blade 13-22, the second stirring blade 13-22 is connected with the stirring shaft 13 through a second telescopic device 13-21 and can realize the distance adjustment of the second stirring blade 13-22 relative to the stirring shaft 13 under the control of a second stirring controller C2; the third stirring assembly 13-3 comprises a third stirring blade 13-32, the third stirring blade 13-32 is connected with the stirring shaft 13 through a third telescopic device 13-31 and can realize the distance adjustment of the third stirring blade 13-32 relative to the stirring shaft 13 under the control of a third stirring controller C3, and the first stirring controller C1, the second stirring controller C2 and the third stirring controller C3 are respectively in signal connection with a master controller C.
Specifically, the external cooling coil 1-2a is spirally wound on the outer wall below the tank bottom support 1-3, so that the overall winding and coating effect of the external cooling coil 1-2a on the reaction tank body 1 is integrally realized.
Specifically, the screw pitch of the outer cooling coils 1-2a of the two adjacent circles is larger than that of the inner cooling coils 1-2b of the two adjacent circles, and the inner housings 1-22 are closer to the reaction tank body 1 and the inner mixture relative to the outer housing 1-21, so that the cooling effect of the inner cooling coils 1-2b relative to the outer cooling coils 1-2a is better, the density and setting requirements of the inner cooling coils 1-2b are relatively higher, the density and setting requirements of the outer cooling coils 1-2a are relatively lower, and the screw pitch of the outer cooling coils 1-2a of the two adjacent circles is larger than that of the inner cooling coils 1-2b of the two adjacent circles.
Specifically, the pipe diameter of the external cooling coil 1-2a is smaller than that of the internal cooling coil 1-2b, and in the cooling process, as the internal shell 1-22 is closer to the reaction tank body 1 and the internal mixture relative to the external shell 1-21, the cooling effect of the internal cooling coil 1-2b is better relative to the external cooling coil 1-2a, the density and setting requirements for the internal cooling coil 1-2b are relatively high, and the density and setting requirements for the external cooling coil 1-2a are relatively low, so that the pipe diameter of the external cooling coil 1-2a is smaller than that of the internal cooling coil 1-2 b.
Specifically, the axial positions of the first stirring assembly 13-1, the second stirring assembly 13-2 and the third stirring assembly 13-3 on the stirring shaft 13 can be adjusted, so that the first stirring assembly 13-1, the second stirring assembly 13-2 and the third stirring assembly 13-3 are arranged at proper axial positions on the stirring shaft 13 according to the mixing reaction requirements of different raw materials.
Specifically, a filter screen assembly 1-22a is further arranged between the tank body shell 1-2 and the tank body bottom support 1-3, so that a finished product meeting the particle size is discharged from the lower part after the mixture after the mixing reaction is filtered, and larger-particle mixture solids which do not meet the conditions are retained above the filter screen assembly 1-22 a.
Specifically, the first stirring vanes 13-12, the second stirring vanes 13-22, and the third stirring vanes 13-32 have the same size, thereby facilitating later replacement and maintenance.
Specifically, the telescopic stroke of the first telescopic device 13-11 is slightly smaller than that of the second telescopic device 13-21, the telescopic stroke of the second telescopic device 13-21 is smaller than that of the third telescopic device 13-31, and in the normal use process, the mixture is gradually filled in the reaction tank body 1 from bottom to top, so that the probability that the mixture is concentrated below the interior of the reaction tank body 1 is certainly greater than the probability that the mixture is concentrated below the interior of the reaction tank body 1, the telescopic stroke of the first telescopic device 13-11 is specifically set to be slightly smaller than that of the second telescopic device 13-21, and the telescopic stroke of the second telescopic device 13-21 is smaller than that of the third telescopic device 13-31, so that the arrangement rule of the mixture in the actual use process is met.
Specifically, a mounting and dismounting flange 13-0 is arranged on the stirring shaft 13 above the first stirring assembly 13-1, so that the connection and fastening between the stirring shaft and the output shaft of the upper driving source are facilitated.
Specifically, the invention also provides a preparation method of phosphite ester by using the reaction kettle, which is characterized in that: the method comprises the following steps:
1) feeding a first raw material and a second raw material into the reaction tank body 1 through a first feeding port 3 and a second feeding port 4 respectively;
2) after the catalyst is fed into the reaction tank body 1 through the stirring shaft inlet 5, the catalyst dosage is less, so that the catalyst can be fed without arranging a special feeding port through the stirring shaft inlet 5, meanwhile, part of the catalyst entering the reaction tank body can be attached to the stirring shaft and each stirring component, the mixing reaction can be carried out with the raw materials along with the rotation of the stirring shaft and each stirring component while the mixing reaction is carried out in the reaction tank body 1, the stirring shaft 13 is connected with the driving source M through the master controller C, the signal connection among the first stirring controller C1 and the first stirring component 13-1, the second stirring controller C2 and the second stirring component 13-2, the third stirring controller C3 and the third stirring component 13-3 is ensured to be smooth, and the first stirring component 13-1, the second stirring component and the third stirring component 13-3 are respectively recorded through the master controller C, The corresponding height positions H1, H2, and H3 of the second stirring assembly 13-2 and the third stirring assembly 13-3;
3) the cooling device comprises an inner coil inlet b-1, an inner cooling coil 1-2b wound on the outer wall of an inner shell 1-22 through the inner coil inlet b-1, an outer coil inlet a-1, an outer cooling coil 1-2a wound on the outer wall of an outer shell 1-21 through the outer coil inlet a-1, an outer coil outlet a-2, and cooling liquid injected into the outer cooling coil 1-2a and the inner cooling coil 1-2b, so that the inner cooling coil 1-2b and the outer cooling coil 1-2a can be conveniently installed, arranged and detached;
4) a driving source M is started to drive the stirring shaft 13 to respectively drive the first stirring component 13-1, the second stirring component 13-2 and the third stirring component 13-3 to synchronously rotate; the material thickness detection device arranged on the inner wall of the inner shell 1-22 detects the axial thickness real-time value H0 of the mixture inside the inner shell 1-22 in real time;
when and only when H0 is more than or equal to H1, which indicates that the mixture is the most at this time, the rotating speed of the stirring shaft needs to be increased to the maximum extent, and the distance between each stirring blade and the stirring shaft 13 is increased so as to realize stirring in a large range through a large radius, the master controller C adjusts the rotating speed of the stirring shaft 13 to be increased from R0 to R1, controls the first stirring blades 13-12 to increase the distance relative to the stirring shaft 13 through the first telescopic devices 13-11 through the first stirring controller C1, controls the second stirring blades 13-22 to increase the distance relative to the stirring shaft 13 through the second telescopic devices 13-21 through the second stirring controller C2, and controls the third stirring blades 13-32 to increase the distance relative to the stirring shaft 13 through the third telescopic devices 13-31 through the third stirring controller C3;
when and only when H1 is greater than H0 and is greater than or equal to H2, which indicates that the mixture is more at the moment, the rotating speed of the stirring shaft needs to be increased to a greater extent, the distance between the stirring blades at corresponding positions and the stirring shaft 13 is increased so as to realize stirring in a large range through a large radius, the total controller C adjusts the rotating speed of the stirring shaft 13 to be increased from R0 to R2, the first stirring controller C1 controls the distance between the first stirring blades 13-12 and the stirring shaft 13 to be unchanged, the second stirring controller C2 controls the second stirring blades 13-22 to be increased through the second expansion devices 13-21 and the third stirring controller C3 controls the distance between the third stirring blades 13-32 and the stirring shaft 13 to be increased through the third expansion devices 13-31;
when H2 is greater than H0 and is greater than or equal to H3, the mixture is slightly more, the rotating speed of the stirring shaft needs to be slightly increased, the distance between the stirring blades at corresponding positions and the stirring shaft 13 is increased to realize stirring in a large range through a large radius, the rotating speed of the stirring shaft 13 is adjusted by the master controller C to be increased from R0 to R3, the distance between the first stirring blades 13-12 and the stirring shaft 13 is controlled to be unchanged through the first stirring controller C1, the distance between the second stirring blades 13-22 and the stirring shaft 13 is controlled to be unchanged through the second stirring controller C2, and the distance between the third stirring blades 13-32 and the stirring shaft 13 is increased through the third telescopic devices 13-31 through the third stirring controller C3;
when and only when H3 is greater than H0, the mixture is few at this time, the rotating speed of the stirring shaft needs to be reduced properly to ensure uniform stirring, meanwhile, the distance between each stirring blade and the stirring shaft 13 does not need to be increased to realize stirring of the mixture in a large range through a large radius, the master controller C keeps the rotating speed of the stirring shaft 13 reduced step by step, meanwhile, the distance between the first stirring blade 13-12 and the stirring shaft 13 is controlled to be unchanged through the first stirring controller C1, the distance between the second stirring blade 13-22 and the stirring shaft 13 is controlled to be unchanged through the second stirring controller C2, and the distance between the third stirring blade 13-32 and the stirring shaft 13 is controlled to be unchanged through the third stirring controller C3;
and R1 > R2 > R3 > R0;
5) keeping the corresponding reaction process for 1-2h within the temperature range of 45-60 ℃, and discharging the obtained product from a lower discharge port 11 after filtering;
6) flash evaporation is carried out in the reaction tank body 1, and the obtained gas product is discharged through an upper vent.
More preferably, the first stirring controller C1 can control the expansion and contraction speed of the first stirring blade 13-12 when it is telescopically adjusted by the first expansion and contraction device 13-11, the second stirring controller C2 can control the expansion and contraction speed of the second stirring blade 13-22 when it is telescopically adjusted by the second expansion and contraction device 13-21, and the third stirring controller C3 can control the expansion and contraction speed of the third stirring blade 13-32 when it is telescopically adjusted by the third expansion and contraction device 13-31, so as to avoid the risk of breakage and damage during the synchronization of rotation and telescopic adjustment due to the excessively fast expansion and contraction speed, and avoid the defect that sufficient mixing and reaction cannot be satisfied due to the excessively slow expansion and contraction speed.
In addition to the above embodiments, the present invention may have other embodiments, which are not described in detail herein. But all the technical solutions formed by equivalent substitutions or equivalent transformations belong to the protection scope of the claims of the present invention.
Claims (10)
1. A phosphite ester preparation method, which is characterized in that: the method comprises the following steps:
1) feeding a first raw material and a second raw material into the reaction tank body (1) through a first feeding port (3) and a second feeding port (4) respectively;
2) after a catalyst is fed into the reaction tank body (1) through the stirring shaft inlet (5), the stirring shaft (13) is connected with the driving source (M) through the master controller (C), signal connection between the first stirring controller (C1) and the first stirring assembly (13-1), between the second stirring controller (C2) and the second stirring assembly (13-2), and between the third stirring controller (C3) and the third stirring assembly (13-3) is confirmed to be smooth, and corresponding height positions H1, H2 and H3 of the first stirring assembly (13-1), the second stirring assembly (13-2) and the third stirring assembly (13-3) are respectively recorded through the master controller (C);
3) respectively winding and arranging an inner cooling coil (1-2 b) on the outer wall of the inner shell (1-22) through an inner coil inlet (b-1), then penetrating out through an inner coil outlet (b-2), winding and arranging an outer cooling coil (1-2 a) on the outer wall of the outer shell (1-21) through an outer coil inlet (a-1), then penetrating out through an outer coil outlet (a-2), and respectively injecting cooling liquid into the outer cooling coil (1-2 a) and the inner cooling coil (1-2 b);
4) a driving source (M) is started to drive a stirring shaft (13) to respectively drive a first stirring component (13-1), a second stirring component (13-2) and a third stirring component (13-3) to synchronously rotate; the material thickness detection device arranged on the inner wall of the inner shell (1-22) detects the axial thickness real-time value H0 of the mixture inside the inner shell (1-22) in real time;
when and only when H0 is larger than or equal to H1, the master controller (C) adjusts the rotating speed of the stirring shaft (13) to be increased from R0 to R1, meanwhile, the first stirring blade (13-12) is controlled by the first stirring controller (C1) to increase the distance relative to the stirring shaft (13) through the first telescopic device (13-11), the second stirring blade (13-22) is controlled by the second stirring controller (C2) to increase the distance relative to the stirring shaft (13) through the second telescopic device (13-21), and the third stirring blade (13-32) is controlled by the third stirring controller (C3) to increase the distance relative to the stirring shaft (13) through the third telescopic device (13-31);
when and only when H1 is more than H0 and more than or equal to H2, the master controller (C) adjusts the rotating speed of the stirring shaft (13) to be increased from R0 to R2, simultaneously controls the distance between the first stirring blades (13-12) and the stirring shaft (13) to be unchanged through the first stirring controller (C1), controls the distance between the second stirring blades (13-22) and the stirring shaft (13) to be increased through the second telescopic devices (13-21) through the second stirring controller (C2), and controls the distance between the third stirring blades (13-32) and the stirring shaft (13) to be increased through the third telescopic devices (13-31) through the third stirring controller (C3);
when and only when H2 is more than H0 and more than or equal to H3, the master controller (C) adjusts the rotating speed of the stirring shaft (13) to be increased from R0 to R3, simultaneously controls the distance between the first stirring blades (13-12) and the stirring shaft (13) to be unchanged through the first stirring controller (C1), controls the distance between the second stirring blades (13-22) and the stirring shaft (13) to be unchanged through the second stirring controller (C2), and controls the distance between the third stirring blades (13-32) and the stirring shaft (13) to be increased through the third telescopic device (13-31) through the third stirring controller (C3);
if and only if H3 > H0, the overall controller (C) keeps the rotation speed of the stirring shaft (13) gradually reduced, and simultaneously controls the distance between the first stirring blades (13-12) and the stirring shaft (13) to be constant through the first stirring controller (C1), controls the distance between the second stirring blades (13-22) and the stirring shaft (13) to be constant through the second stirring controller (C2), and controls the distance between the third stirring blades (13-32) and the stirring shaft (13) to be constant through the third stirring controller (C3);
and R1 > R2 > R3 > R0;
5) keeping the corresponding reaction process for 1-2h within the temperature range of 45-60 ℃, and discharging the obtained product from a lower discharge outlet (11) after filtering;
6) and (3) carrying out flash evaporation in the reaction tank body (1), and discharging the obtained gas product through an upper vent.
2. A phosphite ester reaction tank used in the phosphite ester production method of claim 1, wherein: the device comprises a reaction tank body (1) and a supporting tank body (2), wherein the reaction tank body (1) is supported and arranged above the supporting tank body (2); wherein,
the reaction tank body (1) comprises a tank body top cover (1-1) positioned at the top of the upper portion, a tank body shell (1-2) positioned at the middle portion and a tank body bottom support (1-3) positioned at the bottom of the tank body shell, the tank body shell (1-2) comprises an outer shell (1-21) and an inner shell (1-22), an outer cooling coil (1-2 a) is spirally wound on the outer wall of the outer shell (1-21), an inner cooling coil (1-2 b) is spirally wound on the outer wall of the inner shell (1-22), an outer coil inlet (a-1) is arranged above one side of the outer shell (1-21), an inner coil inlet (b-1), an inner coil outlet (b-2) and a tank body bottom support (1-3) are sequentially arranged on the other side of the outer shell (1-21), And an outer coil outlet (a-2), wherein a material thickness detection device is arranged on the inner wall of the inner shell (1-22);
first pan feeding mouth (3), second pan feeding mouth (4) and (mixing) shaft inlet port (5) have been seted up respectively to jar body top cap (1-1) top, first pan feeding mouth (3), second pan feeding mouth (4) set up respectively in the both sides of (mixing) shaft inlet port (5) jar body top cap (1-1) top is close to one side of first pan feeding mouth (3) still is provided with reserve mouth (6) and sample connection (7) jar body top cap (1-1) top is close to one side of second pan feeding mouth (4) still is provided with blow vent (8) jar body casing (1-2) oblique below the direction of jar body collet (1-3) still inserts and is provided with temperature-detecting device (9) observation window (10) have still been seted up on the outer wall of the supporting jar body (2), and the lower extreme of jar body collet (1-3) stretches out and is provided with bin outlet (11) and via the supporting jar body collet (1-1) The outer wall of the body (2) transversely penetrates out;
a stirring shaft (13) is arranged in the reaction tank body (1) extending from the stirring shaft inlet (5), the stirring shaft (13) is driven by an external driving source (M) to rotate, and the rotation speed control is realized through a master controller (C), a first stirring component (13-1), a second stirring component (13-2) and a third stirring component (13-3) are sequentially arranged on the stirring shaft (13) from top to bottom, wherein the first stirring assembly (13-1) comprises a first stirring blade (13-12), the first stirring blade (13-12) is connected with the stirring shaft (13) through a first telescopic device (13-11) and can realize the distance adjustment of the first stirring blade (13-12) relative to the stirring shaft (13) under the control of a first stirring controller (C1); the second stirring assembly (13-2) comprises a second stirring blade (13-22), the second stirring blade (13-22) is connected with the stirring shaft (13) through a second telescopic device (13-21) and can realize the distance adjustment of the second stirring blade (13-22) relative to the stirring shaft (13) under the control of a second stirring controller (C2); the third stirring assembly (13-3) comprises a third stirring blade (13-32), the third stirring blade (13-32) is connected with the stirring shaft (13) through a third telescopic device (13-31) and can realize the distance adjustment of the third stirring blade (13-32) relative to the stirring shaft (13) under the control of a third stirring controller (C3), and the first stirring controller (C1), the second stirring controller (C2) and the third stirring controller (C3) are respectively in signal connection with the master controller (C).
3. A phosphite reaction kettle according to claim 2, wherein: the outer cooling coil (1-2 a) is also spirally wound on the outer wall below the tank body bottom support (1-3).
4. A phosphite reaction kettle according to claim 2, wherein: the pitch of the outer cooling coil (1-2 a) of two adjacent circles is larger than that of the inner cooling coil (1-2 b) of two adjacent circles.
5. A phosphite reaction kettle according to claim 2, wherein: the pipe diameter of the outer cooling coil (1-2 a) is smaller than that of the inner cooling coil (1-2 b).
6. A phosphite reaction kettle according to claim 2, wherein: the axial positions of the first stirring assembly (13-1), the second stirring assembly (13-2) and the third stirring assembly (13-3) on the stirring shaft (13) can be adjusted.
7. A phosphite reaction kettle according to claim 2, wherein: a filter screen component (1-22 a) is also arranged between the tank body shell (1-2) and the tank body bottom support (1-3).
8. A phosphite reaction kettle according to claim 2, wherein: the first stirring blades (13-12), the second stirring blades (13-22) and the third stirring blades (13-32) have the same size.
9. A phosphite reaction kettle according to claim 2, wherein: the telescopic stroke of the first telescopic device (13-11) is slightly smaller than that of the second telescopic device (13-21), and the telescopic stroke of the second telescopic device (13-21) is slightly smaller than that of the third telescopic device (13-31).
10. A phosphite reaction kettle according to claim 2, wherein: a loading and unloading flange (13-0) is arranged above the first stirring component (13-1) on the stirring shaft (13).
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