CN219111586U - Device for continuously preparing dichloropentaerythritol diphosphite - Google Patents
Device for continuously preparing dichloropentaerythritol diphosphite Download PDFInfo
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Abstract
The utility model provides a device for continuously preparing dichloro pentaerythritol diphosphite, which comprises: the device comprises a pentaerythritol suspension preparation kettle, a phosphorus trichloride storage tank, a premixer, a one-stage or multistage series-connected scraper film reactor and a hydrogen chloride tail gas absorption system; the pentaerythritol suspension preparation kettle and the phosphorus trichloride storage tank are both communicated with the inlet of the premixer, the outlet of the premixer is connected with the inlet of the first-stage scraper film reactor, and the gas phase outlet of the scraper film reactor is connected with the gas inlet of the hydrogen chloride tail gas absorption system. The scheme provided by the utility model has high yield and low energy consumption, and can continuously synthesize the dichloropentaerythritol diphosphite.
Description
Technical Field
The utility model relates to the technical field of chemical equipment, in particular to a device for continuously preparing dichloro pentaerythritol diphosphite.
Background
Dichloro pentaerythritol diphosphite is a key intermediate for synthesizing phosphite antioxidants 618, 626, PEP-36 and the like.
The dichloropentaerythritol diphosphite is synthesized by the reaction of phosphorus trichloride and pentaerythritol, and the reaction equation is as follows:
the reaction process generates a large amount of hydrogen chloride, and the discharge rate and the residual amount of the hydrogen chloride gas affect the conversion rate of the product.
There are two general classes of methods for preparing dichloropentaerythritol bisphosphites: one type is a catalytic reaction, such as: european patent EP0113994 uses phosphate as a catalyst to react phosphorus trichloride with pentaerythritol directly at a temperature of 90-110 ℃. Japanese patent JP5059074 uses methylformamide as a catalyst and phosphorus trichloride is reacted with pentaerythritol in a toluene solvent in an excess of 20%. The other type is a catalytic-free reaction, such as U.S. Pat. No. 3,379, 3192243, wherein chloroform is used as a solvent at normal temperature, and phosphorus trichloride is added into a pentaerythritol suspension of chloroform for reaction for 24-48 hours. Czech patent CS190732 uses toluene as solvent at normal temperature, and dry air or inert gas (such as nitrogen) is blown in during the reaction.
Chinese patent CN1069645C is prepared by slowly adding pentaerythritol into phosphorus trichloride toluene solution system, and reacting at 40-60 ℃ and 5-30mmHg vacuum for 5-10 h.
Chinese patent CN102020677A drops phosphorus trichloride into pentaerythritol suspension of halohydrocarbon at 0-5 ℃, and then heats up to 35-160 ℃ to react for 1-12h to prepare dichloro pentaerythritol diphosphite. The low-temperature dropwise addition is adopted in the early stage, so that the energy consumption is increased, and the discharge of the generated hydrogen chloride gas is not facilitated.
Chinese patent CN108047273A adds phosphorus trichloride into a system of pentaerythritol, organic solvent and organic weak base at 15-20 ℃, carries out two-stage heating reaction at 30-40 ℃ and 110-115 ℃, and vacuum extracts generated hydrogen chloride gas at 110-115 ℃ to prepare the dichloropentaerythritol diphosphite. The low-temperature dropwise addition is adopted in the early stage, so that the energy consumption is increased and the generated hydrogen chloride gas is not easy to discharge; the temperature is raised in the stage, so that side reactions are increased, and the yield is reduced.
In the prior art, a kettle type intermittent process is adopted, the reaction time is longer, and the equipment generation efficiency is low; in order to improve and ensure the conversion rate of products, the kettle type reaction is difficult to quickly and thoroughly discharge hydrogen chloride gas, and adopts the modes of introducing dry air or nitrogen, heating up in complicated stages, vacuumizing and the like to discharge the generated hydrogen chloride as much as possible, thereby bringing the problems of increasing the amount of waste gas, increasing side reactions, increasing energy consumption and the like.
Because pentaerythritol is insoluble in solvents such as toluene and halogenated hydrocarbon, the reaction of pentaerythritol and phosphorus trichloride is a reaction of generating a gas-liquid product through solid-liquid synthesis, the problems that a reactor is blocked or solid materials are piled up in the development of continuous process, the generated hydrogen chloride gas is difficult to timely discharge, the reaction is affected, side reactions are increased and the like exist, and the development difficulty of the continuous process is high. The data are searched, and no continuous synthesis report of the dichloropentaerythritol diphosphite is seen.
Disclosure of Invention
The utility model aims to provide a device for continuously preparing dichloropentaerythritol diphosphite, which solves the problems of the prior art, has high yield and low energy consumption, and can continuously synthesize the dichloropentaerythritol diphosphite.
In order to achieve the above object, the present utility model provides the following solutions:
the utility model provides a device for continuously preparing dichloro pentaerythritol diphosphite, which comprises: the device comprises a pentaerythritol suspension preparation kettle, a phosphorus trichloride storage tank, a premixer, a one-stage or multistage series-connected scraper film reactor and a hydrogen chloride tail gas absorption system; the pentaerythritol suspension preparation kettle and the phosphorus trichloride storage tank are both communicated with the inlet of the premixer, the outlet of the premixer is connected with the inlet of the scraper film reactor of the first stage, and the gas phase outlet of the scraper film reactor is connected with the gas inlet of the hydrogen chloride tail gas absorption system;
when only one stage of the scraper film reactor is arranged, the bottom liquid phase outlet of the scraper film reactor is a synthesized solution outlet of the dichloropentaerythritol diphosphite product;
when the scraper film reactors are arranged in series in multiple stages, a liquid phase outlet at the bottom of the front-stage reactor is connected with an inlet of the rear-stage scraper film reactor; the bottom liquid phase outlet of the final-stage scratch board film reactor is the synthesized solution outlet of the dichloropentaerythritol diphosphite product.
Preferably, a feed liquid distributor is arranged in the scraper film reactor, and an inlet of the scraper film reactor is connected with the feed liquid distributor inside;
and a foam remover is arranged in the scraper film reactor, and hydrogen chloride gas released by reaction is discharged from a gas phase outlet after passing through the foam remover.
Preferably, each stage of the scraper film reactor is correspondingly provided with a condenser and a gas-liquid separator, and a gas phase outlet of the scraper film reactor is connected with the hydrogen chloride tail gas absorption system after passing through the condenser and the gas-liquid separator in sequence; and the liquid phase outlet of the gas-liquid separator is connected with the condensate inlet of the corresponding scraper film reactor.
Preferably, the inlet of the premixer can be connected with the outlet of a phosphorus trichloride feeding pump and/or the outlet of a pentaerythritol suspension feeding pump through a first preheater, the inlet of the pentaerythritol suspension feeding pump is connected with the outlet of the pentaerythritol suspension preparation kettle, and the inlet of the phosphorus trichloride feeding pump is connected with the outlet of the phosphorus trichloride storage tank.
Preferably, the outlet of the pre-mixer is connected with the inlet of the scraper film reactor through a second pre-heater.
Preferably, the pentaerythritol suspension preparation kettle is provided with a heating jacket.
Preferably, when the scraper film reactors are arranged in series in multiple stages, the scraper film reactor at the previous stage is connected with the scraper film reactor at the next stage through a mixer, and the outlet of the phosphorus trichloride feeding pump is connected with the inlet of the mixer.
Preferably, the catalyst preparation device further comprises a catalyst storage tank, wherein the outlet of the catalyst storage tank is communicated with a catalyst feeding pump, and the catalyst feeding pump can pump catalyst into the pentaerythritol suspension preparation kettle and each stage of the scraper film reactor or a certain stage of the scraper film reactor.
Compared with the prior art, the utility model has the following technical effects:
1) The reaction of generating gas-liquid products by solid-liquid synthesis of pentaerythritol and phosphorus trichloride in a solvent is carried out in the scraper film reactor, the reaction is carried out rapidly, and the scraper film reactor can be used for vigorously mixing materials, so that the contact of the reaction materials is increased; the scraper film reactor is very suitable for a solid-liquid reaction system, and the problems of blockage, solid accumulation and the like are avoided; the liquid film layer of the reaction material is very thin, the heat transfer area is large, the heat transfer is fast, and the accurate temperature control is facilitated; the generated hydrogen chloride can be rapidly separated from the membrane layer, so that the reaction in the feed liquid membrane layer is pushed to the right.
2) The feed liquid in the scraper film reactor flows from top to bottom by utilizing gravity, so that back mixing can be well controlled, and side reaction is reduced; the flow direction of the material liquid film layer is opposite to the discharge direction of the hydrogen chloride gas, the closer to the end point is the material, the lower the concentration of the hydrogen chloride in the gas-liquid two phases is, the influence of the hydrogen chloride on the reaction is avoided to the greatest extent, the reaction speed is improved, the occurrence of side reaction is controlled, and the product is obtained in high yield.
3) The reactors connected in series in multiple stages can be heated up by gradient, so that the requirements of accurate control of reaction temperatures in different stages are met.
4) The utility model does not need a huge vacuumizing system, does not need to be introduced with dry air or nitrogen to assist in discharging hydrogen chloride gas, reduces the exhaust emission, can well complete the reaction under micro negative pressure, normal pressure or micro positive pressure, and has good energy-saving and environment-friendly effects.
5) The utility model has the advantages of continuous production process, high equipment utilization rate, high production capacity, easy realization of automatic operation, stable process parameters, low difficulty in amplification of the reactor, high operation elasticity and good guarantee of product yield and quality.
Drawings
In order to more clearly illustrate the embodiments of the present utility model or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present utility model, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural diagram of an apparatus for continuously producing dipentaerythritol dichlorophosphite according to example II;
in the figure: 1-preparing a pentaerythritol suspension liquid preparation kettle; 2-pentaerythritol suspension feed pump; 3-a preheater; 4-phosphorus trichloride storage tank; a 5-phosphorus trichloride feed pump; 6-a premixer; 7-a scratch board thin film reactor; 8-a condenser; 9-a gas-liquid separator; 10-hydrogen chloride tail gas absorption system; 11-a mixer; 12-a catalyst reservoir; 13-catalyst feed pump.
Detailed Description
The following description of the embodiments of the present utility model 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 utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
The utility model aims to provide a device for continuously preparing dichloropentaerythritol diphosphite, which solves the problems of the prior art, has high yield and low energy consumption, and can continuously synthesize the dichloropentaerythritol diphosphite.
In order that the above-recited objects, features and advantages of the present utility model will become more readily apparent, a more particular description of the utility model will be rendered by reference to the appended drawings and appended detailed description.
Example 1
This example provides a method for continuously preparing dichloropentaerythritol bisphosphite comprising the steps of:
step one, mixing pentaerythritol with an organic solvent to obtain a pentaerythritol suspension;
introducing the pentaerythritol suspension and phosphorus trichloride into one-stage or multistage serial scraper film reactors for continuous esterification, discharging the generated HCl gas from the upper part of each stage of scraper film reactor, and gradually flowing the reaction liquid flowing out of the bottoms of the multistage serial scraper film reactors into the next stage of scraper film reactor until the solution of the dichloropentaerythritol diphosphite product is discharged from the bottoms of the scraper film reactors, wherein the esterification temperature is 30-100 ℃.
In this embodiment, the organic solvent preferably includes toluene, xylene, trimethylbenzene, 1, 2-dichloropropane, 1, 3-dichloropropane or 1,2, 3-trichloropropane, more preferably toluene or 1, 2-dichloropropane.
In this embodiment, the molar ratio of pentaerythritol to phosphorus trichloride is preferably 1:2 to 3, more preferably 1;2.2 to 2.5. In the present utility model, the mass ratio of pentaerythritol to the organic solvent is preferably 10 to 20:100, more preferably 15:100.
In this embodiment, the mixed solution obtained by mixing preferably further includes an organic amine catalyst. In the present utility model, the organic amine catalyst is preferably included in one or more of N, N-dimethylaniline, N-dimethyl N-butylamine, N-methylformamide, N-dimethylcyclohexylamine, triethylamine, N-diisopropylethylamine, 4-dimethylaminopyridine or pyridine, more preferably N, N-dimethyl N-butylamine. In the present utility model, the molar ratio of pentaerythritol to the organic amine catalyst is preferably 1:0.01 to 0.50, more preferably 1:0.02 to 0.04.
In this embodiment, the esterification reaction is preferably a classification reaction, and the number of stages of the classification reaction is preferably 1 to 15, more preferably 2 to 10, still more preferably 2 to 7. The utility model preferably limits the temperature of different stages according to the stage number of the classification reaction, introduces the temperature of each stage by taking the stage number of the classification reaction as 1-3 as an example, and when the stage number of the classification reaction is 1 stage, the temperature of the esterification reaction is 30-90 ℃, preferably 50-70 ℃; when the number of stages of the classification reaction is 2, the temperature of the first stage reaction in the esterification reaction is 30-70 ℃, preferably 40-60 ℃, and the temperature of the second stage reaction in the esterification reaction is 40-100 ℃, preferably 50-90 ℃; when the number of stages of the classification reaction is 3, the temperature of the first stage reaction in the esterification reaction is 30 to 80 ℃, preferably 40 to 60 ℃, the temperature of the second stage reaction in the esterification reaction is 40 to 90 ℃, preferably 40 to 80 ℃, and the temperature of the third stage reaction in the esterification reaction is 40 to 100 ℃, preferably 40 to 90 ℃.
The multistage classification reaction is performed at different temperatures in the embodiment, so that hydrogen chloride generated by the reaction is removed, the forward movement of the reaction is promoted, and the yield of the dichloropentaerythritol diphosphite is improved. In the present utility model, as the reaction stage number increases, the reaction temperature increases, so long as the hydrogen chloride formed can be removed.
Wherein, in the multistage series connection of the scraper film reactors, the catalyst is respectively added from the inlet of each stage of the scraper film reactors or from the inlet of a certain stage of the scraper film reactors according to a certain proportion.
In other embodiments, in step two, the pentaerythritol suspension and phosphorus trichloride are premixed by a mixer and then reacted in a scraped film reactor.
In other embodiments, in the second step, pentaerythritol suspension or phosphorus trichloride raw material or feed liquid obtained by mixing pentaerythritol suspension and phosphorus trichloride is preheated to 30-60 ℃ and then enters a scraper film reactor for reaction; the temperature of the mixing is preferably 30 to 60 ℃, more preferably 40 to 50 ℃.
In other embodiments, the reaction temperature in the first stage of the scraper film reactor is 30-80 ℃, the reaction temperature in the second stage of the scraper film reactor is 40-90 ℃, and the reaction temperature in the third stage or more of the scraper film reactors is 40-100 ℃;
in the multistage series-connection scraper film reactors, phosphorus trichloride is divided into a plurality of strands, and the strands enter each stage of scraper film reactor or the first stage and the subsequent part of scraper film reactors respectively to participate in the reaction;
phosphorus trichloride entering each stage of scraper film reactor is mixed with pentaerythritol suspension or material discharged from the previous stage of scraper film reactor by a mixer and then enters the corresponding scraper film reactor;
the reaction pressure in the scraper film reactor is micro negative pressure, normal pressure or micro positive pressure;
HCl gas discharged from each stage of scraper film reactor is condensed by a condenser, separated into gas and liquid, and the like, so as to recover solvent and reactant entrained in gas phase, and the solvent and reactant are returned to the corresponding scraper film reactor;
in other embodiments, the solution of dipentaerythritol dichloridate prepared by the first-stage scraped film reactor may be returned to the scraped film reactor inlet and mixed with the incoming pentaerythritol suspension and phosphorus trichloride for cyclic reaction until the desired conversion is reached.
Example two
The embodiment provides a device for continuously preparing the dichloropentaerythritol diphosphite, which is used for realizing the method for continuously preparing the dichloropentaerythritol diphosphite in the embodiment one, and comprises a pentaerythritol suspension preparation kettle 1, a phosphorus trichloride storage tank 4, a premixer 6, a one-stage or multistage series-connection scraper film reactor 7 and a hydrogen chloride tail gas absorption system 10, as shown in figure 1;
wherein, the pentaerythritol suspension preparation kettle 1 is used for preparing pentaerythritol suspension, the phosphorus trichloride storage tank 4 is used for storing phosphorus trichloride, the pentaerythritol suspension preparation kettle 1 is provided with an organic solvent adding port and a pentaerythritol adding port, and the pentaerythritol suspension is prepared by using an organic solvent and pentaerythritol; in the preferred embodiment, a feed liquid distributor is arranged in the scraper film reactor 7, and the inlet of the scraper film reactor 7 is connected with the feed liquid distributor inside; the scraper film reactor 7 is internally provided with a foam remover, and hydrogen chloride gas released by the reaction is discharged from a gas phase outlet after passing through the foam remover. In a preferred embodiment, pentaerythritol suspension formulation tank 1 is provided with a heating jacket to facilitate adjustment of the formulation temperature of the suspension; the pentaerythritol suspension preparation kettle 1 and the phosphorus trichloride storage tank 4 are both communicated with the inlet of the premixer 6, the outlet of the premixer 6 is connected with the inlet of the first-stage scraper film reactor 7, and the gas-phase outlet of the scraper film reactor 7 is connected with the gas inlet of the hydrogen chloride tail gas absorption system 10; pumping the pentaerythritol suspension in the pentaerythritol suspension preparation kettle 1 into a premixer 6 through a pentaerythritol suspension feeding pump 2; pumping the phosphorus trichloride in the phosphorus trichloride storage tank 4 into a premixer 6 through a phosphorus trichloride feeding pump 5;
the reaction of generating gas-liquid products by solid-liquid synthesis of pentaerythritol and phosphorus trichloride in a solvent is carried out in the scraper film reactor 7, the reaction is carried out rapidly, and the scraper film reactor 7 can carry out severe mixing on materials, so that the contact of the reaction materials is increased; the scraper film reactor 7 is very suitable for a solid-liquid reaction system, and the problems of blockage, solid accumulation and the like are avoided; the liquid film layer of the reaction material is very thin, the heat transfer area is large, the heat transfer is fast, and the accurate temperature control is facilitated; the generated hydrogen chloride can be rapidly separated from the membrane layer, so that the reaction in the feed liquid membrane layer is pushed to the right. The feed liquid in the scraper film reactor 7 flows from top to bottom by utilizing gravity, so that back mixing can be well controlled, and side reaction is reduced; the flow direction of the material liquid film layer is opposite to the discharge direction of the hydrogen chloride gas, the closer to the end point is the material, the lower the concentration of the hydrogen chloride in the gas-liquid two phases is, the influence of the hydrogen chloride on the reaction is avoided to the greatest extent, the reaction speed is improved, the occurrence of side reaction is controlled, and the product is obtained in high yield.
The pentaerythritol suspension and phosphorus trichloride enter one-stage or multi-stage series-connection scraper film reactors 7 to carry out continuous reaction, the generated hydrogen chloride gas is discharged from the upper part of each stage of scraper film reactor 7, and the generated dichloro pentaerythritol diphosphite synthetic solution flows out from the bottom of each stage of scraper film reactor 7. The reaction liquid flowing out from the bottom of the multistage series-connection scraper film reactor 7 gradually enters the inlet of the next stage reactor until the dichloropentaerythritol diphosphite product solution is discharged from the bottom of the final stage reactor.
When only the first-stage scraper film reactor 7 is arranged, the bottom liquid phase outlet of the scraper film reactor 7 is a synthesized solution outlet of the dichloropentaerythritol diphosphite product;
when the multistage series-connection scraper film reactor 7 is arranged, the bottom liquid phase outlet of the former stage reactor is connected with the inlet of the latter stage scraper film reactor 7; the bottom liquid phase outlet of the final-stage scratch film reactor 7 is the synthesized solution outlet of the dichloropentaerythritol diphosphite product. The front-stage scraper film reactor 7 is connected with the next-stage scraper film reactor 7 through a mixer 11, the outlet of a phosphorus trichloride feeding pump 5 is connected with the inlet of the mixer 11, and phosphorus trichloride is divided into a plurality of strands and respectively enters each stage of reactor or the first stage and the subsequent partial reactors to participate in the reaction, wherein the phosphorus trichloride is mixed with pentaerythritol suspension or the materials discharged from the previous stage of reactor through the mixer 11 and then enters the corresponding reactor. The reactors connected in series in multiple stages can be heated up by gradient, so that the requirements of accurate control of reaction temperatures in different stages are met. The number of the stages of the scraper film reactor 7 connected in series is 2-15, preferably 2-10, and more preferably 2-7. The reaction pressure in the scraper film reactor 7 is micro negative pressure, normal pressure or micro positive pressure, preferably micro negative pressure. The reaction temperature in the first stage reactor is preferably 30-80 ℃, more preferably 40-60 ℃, the reaction temperature in the second stage reactor is preferably 40-90 ℃, more preferably 40-80 ℃, and the reaction temperature in the third stage and above reactors is preferably 40-100 ℃, more preferably 40-90 ℃.
In addition, in order to increase the synthesis rate, a catalyst storage tank 12 is further arranged, the outlet of the catalyst storage tank 12 is communicated with a catalyst feeding pump 13, and the catalyst feeding pump 13 can pump catalyst into the pentaerythritol suspension preparation kettle 1 and each stage of scraper film reactor 7 or a certain stage of scraper film reactor 7, and the catalyst is respectively added from the inlet of each stage of reactor or from the inlet of a certain stage of reactor according to a certain proportion.
The utility model does not need a huge vacuumizing system, does not need to be filled with dry air or nitrogen to assist the discharge of hydrogen chloride gas, reduces the exhaust emission, can well complete the reaction under micro negative pressure, normal pressure or micro positive pressure, has good energy-saving and environment-friendly effects, and has continuous production process, high equipment utilization rate, large production capacity, easy realization of automatic operation, stable process parameters, low amplification difficulty of a reactor, high operation elasticity and good guarantee of product yield and quality.
In some embodiments, each stage of scraper film reactor 7 is correspondingly provided with a condenser 8 and a gas-liquid separator 9, and the gas phase outlet of the scraper film reactor 7 is sequentially connected with a hydrogen chloride tail gas absorption system 10 after passing through the condenser 8 and the gas-liquid separator 9; the liquid phase outlet of the gas-liquid separator 9 is connected with the condensate inlet of the corresponding scraper film reactor 7. The hydrogen chloride gas pumped out from the gas phase outlet at the upper part of each stage of scraper film reactor 7 is condensed by a condenser 8 and the solvent and reaction materials carried out are captured by a gas-liquid separator 9, and then enter a hydrogen chloride tail gas absorption system 10. The liquid captured by the gas-liquid separator 9 returns to the corresponding reactor to return to the reaction system, so that the waste of raw materials is reduced.
In some embodiments, the inlet of the premixer 6 may be connected to the outlet of the phosphorus trichloride feed pump 5 and/or the outlet of the pentaerythritol suspension feed pump 2 via the first preheater 3, the inlet of the pentaerythritol suspension feed pump 2 being connected to the outlet of the pentaerythritol suspension preparation tank 1, and the inlet of the pentaerythritol suspension feed pump 2 being connected to the outlet of the phosphorus trichloride tank 4. The first preheater 3 is used for preheating the materials and discharging the materials to the premixer 6.
The outlet of the pre-mixer 6 is connected with the inlet of the scraper film reactor 7 through the second pre-heater 3, and the second pre-heater 3 is used for pre-heating materials and then discharging the materials to the scraper film reactor 7; the pentaerythritol suspension, or the phosphorus trichloride raw material, or the feed liquid obtained by mixing the pentaerythritol suspension and the phosphorus trichloride is preheated to 30-60 ℃ and then enters the scraper film reactor 7 for reaction.
Specific application examples are as follows:
example 1: toluene and pentaerythritol are prepared into a pentaerythritol suspension with 15 wt% in a pentaerythritol suspension preparation kettle, the pentaerythritol suspension is conveyed by a pump and preheated to 50 ℃ by a preheater, the pentaerythritol suspension and phosphorus trichloride are mixed in the premixer and then enter a 3-stage serial scraper film reactor for reaction, the molar ratio of the pentaerythritol to the phosphorus trichloride is 1.0:2.2, the reaction temperature of the first-stage reactor is 50-55 ℃, the reaction temperature of the second-stage reactor is 60-65 ℃, the reaction temperature of the third-stage reactor is 75-85 ℃, and the synthesized solution of the dichloropentaerythritol bisphosphite product is discharged from the bottom of the third-stage reactor. The pressure in the reactor is kept at micro negative pressure by the suction of the hydrogen chloride tail gas absorption system, and hydrogen chloride gas pumped out from a gas phase outlet at the upper part of each stage of the reactor is condensed by a condenser and the solvent and reaction materials carried out are captured by a gas-liquid separator and then enter the hydrogen chloride tail gas absorption system. The liquid trapped by the gas-liquid separator returns to the corresponding reactor to return to the reaction system.
The solution of the dichloropentaerythritol diphosphite product is analyzed, the conversion rate of pentaerythritol is 91.73 percent, and the selectivity of the dichloropentaerythritol diphosphite is 95.35 percent.
Example 2: toluene and pentaerythritol are prepared into a pentaerythritol suspension with 15 wt% in a pentaerythritol suspension preparation kettle, the pentaerythritol suspension is conveyed by a pump and preheated to 50 ℃ by a preheater, the pentaerythritol suspension and phosphorus trichloride are mixed in the premixer and then enter a 5-stage series scraper film reactor for reaction, the molar ratio of the pentaerythritol to the phosphorus trichloride is 1.0:2.2, the reaction temperature of the first-stage reactor is 50-55 ℃, the reaction temperature of the second-stage reactor and the reaction temperature of the third-stage reactor are 60-65 ℃, the reaction temperature of the fourth-stage reactor is 70-75 ℃, the reaction temperature of the fifth-stage reactor is 75-85 ℃, and the synthesized dichloropentaerythritol diphosphite product solution is discharged from the bottom of the fifth-stage reactor. The pressure in the reactor is kept at micro negative pressure by the suction of the hydrogen chloride tail gas absorption system, and hydrogen chloride gas pumped out from a gas phase outlet at the upper part of each stage of the reactor is condensed by a condenser and the solvent and reaction materials carried out are captured by a gas-liquid separator and then enter the hydrogen chloride tail gas absorption system. The liquid trapped by the gas-liquid separator returns to the corresponding reactor to return to the reaction system.
The solution of the dichloropentaerythritol diphosphite product is analyzed, the conversion rate of pentaerythritol is 95.22%, and the selectivity of the dichloropentaerythritol diphosphite is 96.63%.
Example 3:1, 2-dichloropropane, pentaerythritol and a catalyst N, N-dimethyl N-butylamine are prepared into a pentaerythritol suspension with 15%wt in a pentaerythritol suspension preparation kettle, the pentaerythritol suspension is conveyed by a pump and preheated to 40 ℃ by a preheater, the pentaerythritol suspension and phosphorus trichloride are mixed in the premixer and then enter a 4-stage series scraping plate film reactor for reaction, the molar ratio of the pentaerythritol to the phosphorus trichloride to the catalyst is 1.0:2.2:0.02, the reaction temperature of the first-stage reactor is 40-45 ℃, the reaction temperature of the second-stage reactor is 45-50 ℃, the reaction temperature of the third-stage reactor is 55-60 ℃, the reaction temperature of the fourth-stage reactor is 60-65 ℃, and the synthesized dichloropentaerythritol diphosphite product solution is discharged from the bottom of the fourth-stage reactor. The pressure in the reactor is kept at micro negative pressure by the suction of the hydrogen chloride tail gas absorption system, and hydrogen chloride gas pumped out from a gas phase outlet at the upper part of each stage of the reactor is condensed by a condenser and the solvent and reaction materials carried out are captured by a gas-liquid separator and then enter the hydrogen chloride tail gas absorption system. The liquid trapped by the gas-liquid separator returns to the corresponding reactor to return to the reaction system.
The solution of the dichloropentaerythritol diphosphite product is analyzed, the conversion rate of pentaerythritol is 93.55 percent, and the selectivity of the dichloropentaerythritol diphosphite is 97.45 percent.
Example 4: toluene and pentaerythritol are prepared into a pentaerythritol suspension with 15 percent by weight in a pentaerythritol suspension preparation kettle, the pentaerythritol suspension is conveyed by a pump and preheated to 50 ℃ by a preheater, mixed with 60 percent of phosphorus trichloride in a premixer, then the mixture enters a 5-stage series-connection scraper film reactor for reaction, 30 percent of phosphorus trichloride and materials discharged from the bottom of a first-stage reactor are mixed in the mixer and then enter a second-stage reactor for reaction, and 10 percent of phosphorus trichloride and materials discharged from the bottom of the second-stage reactor are mixed in the mixer and then enter a third-stage reactor for reaction. The molar ratio of the reaction of the pentaerythritol and the phosphorus trichloride is 1.0:2.2, the reaction temperature of the first-stage reactor is 50-55 ℃, the reaction temperature of the second-stage reactor and the third-stage reactor is 60-65 ℃, the reaction temperature of the fourth-stage reactor is 70-75 ℃, the reaction temperature of the fifth-stage reactor is 75-85 ℃, and the synthesized solution of the dichloropentaerythritol bisphosphite product is discharged from the bottom of the fifth-stage reactor. The pressure in the reactor is kept at micro negative pressure by the suction of the hydrogen chloride tail gas absorption system, and hydrogen chloride gas pumped out from a gas phase outlet at the upper part of each stage of the reactor is condensed by a condenser and the solvent and reaction materials carried out are captured by a gas-liquid separator and then enter the hydrogen chloride tail gas absorption system. The liquid trapped by the gas-liquid separator returns to the corresponding reactor to return to the reaction system.
The solution of the dichloropentaerythritol diphosphite product is analyzed, the conversion rate of pentaerythritol is 92.35 percent, and the selectivity of the dichloropentaerythritol diphosphite is 96.88 percent.
The principles and embodiments of the present utility model have been described in detail with reference to specific examples, which are provided to facilitate understanding of the method and core ideas of the present utility model; also, it is within the scope of the present utility model to be modified by those of ordinary skill in the art in light of the present teachings. In view of the foregoing, this description should not be construed as limiting the utility model.
Claims (8)
1. A device for continuously preparing dichloro pentaerythritol diphosphite is characterized in that: comprising the following steps: the device comprises a pentaerythritol suspension preparation kettle, a phosphorus trichloride storage tank, a premixer, a one-stage or multistage series-connected scraper film reactor and a hydrogen chloride tail gas absorption system; the pentaerythritol suspension preparation kettle and the phosphorus trichloride storage tank are both communicated with the inlet of the premixer, the outlet of the premixer is connected with the inlet of the scraper film reactor of the first stage, and the gas phase outlet of the scraper film reactor is connected with the gas inlet of the hydrogen chloride tail gas absorption system;
when only one stage of the scraper film reactor is arranged, the bottom liquid phase outlet of the scraper film reactor is a synthesized solution outlet of the dichloropentaerythritol diphosphite product;
when the scraper film reactors are arranged in series in multiple stages, a liquid phase outlet at the bottom of the front-stage reactor is connected with an inlet of the rear-stage scraper film reactor; the bottom liquid phase outlet of the final-stage scratch board film reactor is the synthesized solution outlet of the dichloropentaerythritol diphosphite product.
2. The apparatus for continuously preparing dichloropentaerythritol diphosphite according to claim 1, wherein: the scraper film reactor is internally provided with a feed liquid distributor, and an inlet of the scraper film reactor is connected with the feed liquid distributor inside;
and a foam remover is arranged in the scraper film reactor, and hydrogen chloride gas released by reaction is discharged from a gas phase outlet after passing through the foam remover.
3. The apparatus for continuously preparing dichloropentaerythritol diphosphite according to claim 1, wherein: the scraper film reactor of each stage is correspondingly provided with a condenser and a gas-liquid separator, and a gas phase outlet of the scraper film reactor is connected with the hydrogen chloride tail gas absorption system after passing through the condenser and the gas-liquid separator in sequence; and the liquid phase outlet of the gas-liquid separator is connected with the condensate inlet of the corresponding scraper film reactor.
4. The apparatus for continuously preparing dichloropentaerythritol diphosphite according to claim 1, wherein: the inlet of the premixer can be connected with the outlet of a phosphorus trichloride feeding pump and/or the outlet of a pentaerythritol suspension feeding pump through a first preheater, the inlet of the pentaerythritol suspension feeding pump is connected with the outlet of the pentaerythritol suspension preparation kettle, and the inlet of the phosphorus trichloride feeding pump is connected with the outlet of the phosphorus trichloride storage tank.
5. The apparatus for continuously preparing dichloropentaerythritol diphosphite according to claim 1, wherein: the outlet of the pre-mixer is connected with the inlet of the scraper film reactor through a second pre-heater.
6. The apparatus for continuously preparing dichloropentaerythritol diphosphite according to claim 1, wherein: the pentaerythritol suspension is prepared with a heating jacket.
7. The apparatus for continuously preparing dichloropentaerythritol diphosphite according to claim 4, wherein: when the scraper film reactors are arranged in series in multiple stages, the scraper film reactor at the previous stage is connected with the scraper film reactor at the next stage through a mixer, and the outlet of the phosphorus trichloride feeding pump is connected with the inlet of the mixer.
8. The apparatus for continuously preparing dichloropentaerythritol diphosphite according to claim 7, wherein: the catalyst storage tank is communicated with a catalyst feeding pump, and the catalyst feeding pump can pump catalyst into the pentaerythritol suspension preparation kettle, each stage of the scraper film reactor or a certain stage of the scraper film reactors.
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