CN114832752A - Method and device for continuously synthesizing alkyl phosphate by using microchannel reactor - Google Patents

Method and device for continuously synthesizing alkyl phosphate by using microchannel reactor Download PDF

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CN114832752A
CN114832752A CN202210570634.5A CN202210570634A CN114832752A CN 114832752 A CN114832752 A CN 114832752A CN 202210570634 A CN202210570634 A CN 202210570634A CN 114832752 A CN114832752 A CN 114832752A
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metering pump
microchannel reactor
phosphate
reaction
liquid intermediate
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马航
李云东
刘晨曦
万邦隆
梅连平
朱境
陆忠海
张振环
杨晓龙
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Yunnan Yuntianhua Co Ltd
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Yunnan Yuntianhua Co Ltd
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    • 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
    • B01J4/02—Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
    • 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
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    • C07F9/02—Phosphorus compounds
    • C07F9/06—Phosphorus compounds without P—C bonds
    • C07F9/08—Esters of oxyacids of phosphorus
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    • C07F9/11—Esters of phosphoric acids with hydroxyalkyl compounds without further substituents on alkyl
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    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00851—Additional features
    • B01J2219/00867—Microreactors placed in series, on the same or on different supports
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract

The invention discloses a method and a device for continuously synthesizing alkyl phosphate by using a microchannel reactor, relating to the field of chemical industry. The solid feeding of the micro reaction device is realized by arranging the screw conveyer on the micro reaction device, the large specific surface area of the micro channel reaction device is fully utilized, so that the solid material can be reacted by the microchannel reaction device with improved reaction efficiency, good rapid mixing effect, good heat transfer effect, high temperature and high pressure resistance and the like, the reaction is more sufficient and controllable, the distribution of the raw materials and the products is more optimized and controllable by controlling the reaction temperature and the reaction time of the microchannel reactor, the phosphate, the solid phosphorus pentoxide, the catalyst and the ethylene oxide can enter the microchannel reactor in proportion for reaction by detecting the pumping pressure of the metering pump and adjusting the flow rate of the metering pump, so that the occurrence of side reactions is greatly reduced, the continuous, safe, efficient and stable production of the alkyl phosphate is realized, and the purity of the synthesized alkyl phosphate is obviously improved.

Description

Method and device for continuously synthesizing alkyl phosphate by using microchannel reactor
Technical Field
The invention relates to the field of chemical industry, in particular to a method for continuously synthesizing alkyl phosphate by using a microchannel reactor and a device for continuously synthesizing alkyl phosphate by using the microchannel reactor.
Background
The alkyl phosphate is an important phosphorus-containing additive, has good abrasion resistance and oxidation resistance, and has good composite use performance when being used with a sulfur-series antiwear agent. Meanwhile, alkyl phosphate plays a very important role in the preparation of pesticide organic phosphorus-containing corrosion inhibitors, plastic additives, dye additives and flame retardants, and is an important fine chemical intermediate. When the alkyl phosphate is synthesized, the reaction is violent, a large amount of heat can be released in the reaction process, most of the alkyl phosphate is reacted by a traditional batch reaction kettle at present, the heat exchange area is small, the heat exchange capacity is low, the stable temperature control effect is poor, and the temperature runaway risk is high; the device has a plurality of dead angles, and the process control is in an intermittent fluctuation type state, so that the stability is low and the safety is poor. Compared with the traditional batch type reaction kettle, the micro-channel reactor has the characteristics of small volume, large specific surface area, easy amplification, continuous process, good quick mixing effect, good heat transfer effect, high temperature and high pressure resistance and the like, and the adoption of the continuous flow tubular reactor with a specific structure can effectively control the mixing, mass transfer and heat transfer processes of reaction materials, but the existing micro-channel reactor is only applied to the reaction of which the raw materials are liquid, and the reaction involving solid participation in the synthesis of alkyl phosphates is difficult to realize for the existing micro-reactor.
Disclosure of Invention
The invention aims to provide a method and a device for continuously synthesizing alkyl phosphate by using a microchannel reactor, which solve the problems of low heat exchange capacity, low stability and poor safety of the traditional batch type reaction kettle type production process.
In a first aspect, the present invention provides a method for continuously synthesizing alkyl phosphate ester using a microchannel reactor, comprising the steps of:
s1: conveying the solid phosphorus pentoxide to a first microchannel reactor by a screw conveyor;
s2: feeding phosphate to the first microchannel reactor by a first metering pump;
s3: reacting the solid phosphorus pentoxide and the phosphate in the first microchannel reactor to obtain a first liquid intermediate material;
s4: feeding the first liquid intermediate material to a second microchannel reactor through a second metering pump;
s5: sending alkylene oxide to the second microchannel reactor via a third metering pump;
s6: reacting the first liquid intermediate material with the alkylene oxide in the second microchannel reactor to obtain a second liquid intermediate material;
s7: and (4) sending the second liquid to a collecting tank through a fourth metering pump, carrying out reduced pressure rectification, and collecting fractions to obtain the alkyl phosphate.
In some embodiments, the phosphate ester comprises any one or more of trimethyl phosphate, triethyl phosphate, tripropyl phosphate, tributyl phosphate and dimethyl methyl phosphate.
In some embodiments, the alkylene oxide comprises any one or more of ethylene oxide, propylene oxide, and pentane oxide.
In some embodiments, the step S2 of feeding the phosphate ester to the first microchannel reactor by the first metering pump includes: mixing the phosphate with a catalyst in proportion to obtain mixed phosphate; the mixed phosphate ester is pumped through the first metering pump to the first microchannel reactor.
In some embodiments, the catalyst comprises titanium oxide acetylacetonate, alpha stannous, stannous octoate, solid pyrophosphoric acid, C 2 H 5 Any one or more of ONa.
In some embodiments, the molar ratio of the phosphate ester, the solid phosphorus pentoxide, the catalyst, and the alkylene oxide is 1: 0.51-0.16: 0.012-0.22: 0.535-0.63.
In some embodiments, the molar ratio of the phosphate ester, solid phosphorus pentoxide, catalyst, and alkylene oxide is 1:0.55:0.016: 0.58.
In some embodiments, the pumping flow rate of the second metering pump is from 25ml/min to 35ml/min and the pumping flow rate of the third metering pump is from 10ml/min to 20 ml/min.
In some embodiments, the pumping flow rate of the second metering pump is from 32ml/min to 35ml/min and the pumping flow rate of the third metering pump is from 14ml/min to 18 ml/min.
In some embodiments, the step S3, reacting the solid phosphorus pentoxide and the phosphate ester in the first microchannel reactor to obtain a first liquid intermediate material, includes: preheating the solid phosphorus pentoxide and the phosphate ester; and reacting the preheated solid phosphorus pentoxide and the phosphate in the first microchannel reactor to obtain a first liquid intermediate material.
In some embodiments, in step S6, reacting the first liquid intermediate material and the alkylene oxide in the second microchannel reactor to obtain a second liquid intermediate material, comprising: preheating the first liquid intermediate stream and the alkylene oxide; and reacting the preheated first liquid intermediate material and the alkylene oxide in the second microchannel reactor to obtain a second liquid intermediate material.
In some embodiments, the method for continuously synthesizing alkyl phosphate ester using a microchannel reactor further comprises: detecting pumping pressures of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump to obtain pressure data; and adjusting the pumping flow rates of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump based on the pressure data.
In some embodiments, the method for continuously synthesizing alkyl phosphate ester using a microchannel reactor further comprises: detecting the reaction temperature of the first microchannel reactor and the second microchannel reactor to obtain temperature data; and adjusting the pumping flow rates of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump based on the temperature data.
In some embodiments, the reaction temperature is 40-60 ℃ and the reaction time is 10-30min in step S3, and the reaction temperature is 80-120 ℃ and the reaction time is 60-300S in step S6.
In some embodiments, the reaction temperature is 45-55 ℃ and the reaction time is 15-25min in the step S3, and the reaction temperature is 95-105 ℃ and the reaction time is 120-240S in the step S6.
In a second aspect, the present invention provides an apparatus for continuously synthesizing alkyl phosphate using a microchannel reactor, comprising: the screw conveyer is connected with the first micro-channel reactor and is used for conveying the solid phosphorus pentoxide to the first micro-channel reactor; the first metering pump is connected with the first microchannel reactor and is used for pumping the phosphate to the first microchannel reactor; a first microchannel reactor for reacting the solid phosphorus pentoxide with the phosphate ester to obtain a first liquid intermediate material; the second metering pump is connected with the second micro-channel reactor and is used for pumping the first liquid intermediate material to the second micro-channel reactor; a third metering pump connected to the second microchannel reactor for pumping alkylene oxide to the second microchannel reactor; a second microchannel reactor for reacting the first liquid intermediate material with the alkylene oxide to obtain a second liquid intermediate material; the fourth metering pump is connected with the collecting tank and is used for pumping the second liquid intermediate material to the collecting tank; and the collecting tank is used for carrying out reduced pressure rectification on the second liquid intermediate material, and collecting fractions to obtain the alkyl phosphate.
In some embodiments, the first microchannel reactor and the second microchannel reactor are hermetically sealed.
In some embodiments, the apparatus for continuously synthesizing alkyl phosphate using a microchannel reactor further comprises: the pressure sensors are respectively arranged on the first metering pump, the second metering pump, the third metering pump and the fourth metering pump and are used for detecting the pumping pressures of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump to obtain pressure data; adjusting pumping flow rates of the first, second, third, and fourth metering pumps based on the pressure data.
In some embodiments, the apparatus for continuously synthesizing alkyl phosphate using a microchannel reactor further comprises: the temperature sensors are respectively arranged on the first microchannel reactor and the second microchannel reactor and are used for detecting the reaction temperatures of the first microchannel reactor and the second microchannel reactor to obtain temperature data; and adjusting the pumping flow rates of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump.
In some embodiments, the apparatus for continuously synthesizing alkyl phosphate using a microchannel reactor further comprises: and the screening device is used for screening the solid phosphorus pentoxide, wherein the undersize fine-particle phosphorus pentoxide which passes through the screening device enters the first microchannel reactor.
In some embodiments, the first microchannel reactor comprises: a first preheating section and a first reaction section; the second microchannel reactor comprises: a second preheating section and a second reaction section; the spiral conveyor and the first metering pump are respectively connected with the first preheating section, the first preheating section is connected with the first reaction section, the second metering pump and the third metering pump are respectively connected with the second preheating section, and the second preheating section is connected with the second reaction section.
In some embodiments, the first and second preheating stages are a straight manifold structure; the first reaction section and the second reaction section are of pulse variable-diameter structures.
Compared with the prior art, the invention has the beneficial effects that:
the solid feeding of the micro reaction device is realized by arranging the screw conveyer on the micro reaction device, the specific surface area of the micro channel reaction device is fully utilized, the solid material can improve the reaction efficiency through the micro channel reaction device, the rapid mixing effect is good, the heat transfer effect is good, the high temperature and high pressure resistance and other characteristics are realized, the reaction is more sufficient and controllable, the reaction temperature and the reaction time of the micro channel reactor are controlled, the distribution of raw materials and products is more optimized and controllable, phosphate can be realized by detecting the pumping pressure of the metering pump and adjusting the flow rate of the metering pump, solid phosphorus pentoxide, catalyst and ethylene oxide enter the micro channel reactor in proportion for reaction, and the occurrence of side reactions is greatly reduced. Compared with the traditional batch production method, the method has incomparable advantages, provides an important way for improving the industrial continuous production of the phosphate, realizes the continuous, safe, efficient and stable production of the alkyl phosphate, and obviously improves the purity of the synthesized alkyl phosphate.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as claimed.
Drawings
FIG. 1 shows a schematic flow diagram of a continuous process for the synthesis of alkyl phosphate esters using a microchannel reactor according to the present invention;
FIG. 2 is a schematic flow diagram showing a continuous process for the synthesis of alkyl phosphate esters using a microchannel reactor according to another embodiment of the present invention;
FIG. 3 shows a schematic flow diagram of a continuous process for the synthesis of alkyl phosphate esters using a microchannel reactor according to another embodiment of the present invention;
FIG. 4 shows a schematic flow diagram of a continuous process for the synthesis of alkyl phosphate esters using a microchannel reactor according to another embodiment of the present invention;
FIG. 5 is a schematic flow diagram showing a continuous process for the synthesis of alkyl phosphate esters using a microchannel reactor according to another embodiment of the present invention;
FIG. 6 is a schematic flow diagram showing a continuous process for the synthesis of alkyl phosphate esters using a microchannel reactor according to another embodiment of the present invention;
FIG. 7 is a schematic diagram showing the structure of an apparatus for continuously synthesizing alkyl phosphate ester using a microchannel reactor according to the present invention;
FIG. 8 shows a schematic diagram of a microchannel structure of an apparatus for continuously synthesizing alkyl phosphate ester using a microchannel reactor according to the present invention: the pulse diameter-changing structure comprises a-a direct current shape structure, b-a diamond pulse diameter-changing structure, c-a heart-shaped pulse diameter-changing structure and d-a circular pulse diameter-changing structure.
Detailed Description
The disclosure will now be discussed with reference to several exemplary embodiments. It is to be understood that these examples are discussed only to enable those of ordinary skill in the art to better understand and thus implement the teachings of the present invention, and are not meant to imply any limitations on the scope of the invention.
As used herein, the term "include" and its variants are to be read as open-ended terms meaning "including, but not limited to. The term "based on" is to be read as "based, at least in part, on". The terms "one embodiment" and "an embodiment" are to be read as "at least one embodiment". The term "another embodiment" is to be read as "at least one other embodiment".
In the prior production of flame retardant, alkyl phosphate is an important phosphorus-containing additive, most of the alkyl phosphate synthesized at present is reacted by a traditional batch reaction kettle, but the heat exchange area is small, the heat exchange capability is low, the temperature control effect is poor, meanwhile, the batch type reaction kettle is in a batch fluctuation type state when in work, the stability is low, the safety is poor, compared with the traditional batch type reaction kettle, the microchannel reactor has the characteristics of small volume, large specific surface area, easy amplification, continuous process, good rapid mixing effect, good heat transfer effect, high temperature and high pressure resistance and the like, and the mass transfer and heat transfer processes of the reaction materials and the synthesis of the alkyl phosphate can be effectively controlled by using a micro reaction device, however, it is difficult to realize a micro-reactor at present when the reaction involving solid participation is involved in the synthesis of alkyl phosphates.
In order to solve the above problems, as shown in fig. 1, an embodiment of the present invention provides a method for continuously synthesizing alkyl phosphate ester using a microchannel reactor, which may include the steps of: s1: conveying the solid phosphorus pentoxide to a first microchannel reactor by a screw conveyor; s2: feeding phosphate to a first microchannel reactor through a first metering pump; s3: reacting solid phosphorus pentoxide and phosphate in a first microchannel reactor to obtain a first liquid intermediate material; s4: feeding the first liquid intermediate material to a second microchannel reactor through a second metering pump; s5: sending the alkylene oxide to a second microchannel reactor by a third metering pump; s6: reacting the first liquid intermediate material with the alkylene oxide in a second microchannel reactor to obtain a second liquid intermediate material; s7: and (4) sending the second liquid to a collecting tank through a fourth metering pump, carrying out reduced pressure rectification, and collecting fractions to obtain the alkyl phosphate. The method is a continuous synthesis method, so that raw materials are fully reacted, the high-efficiency mass transfer and heat transfer efficiency of the microchannel reactor is utilized, the mass transfer rate among three-phase materials of solid phosphorus pentoxide, liquid phosphate and gas alkylene oxide is effectively enhanced, and the safety and operability of experiments are greatly improved.
In some embodiments, the phosphate ester may include any one or more of trimethyl phosphate, triethyl phosphate, tripropyl phosphate, tributyl phosphate and dimethyl methyl phosphate. The phosphate ester is an ester derivative of phosphoric acid, belongs to the class of phosphoric acid derivatives, and is a tribasic acid which is a main raw material for generating alkyl phosphate ester.
In some embodiments, the alkylene oxide may include any one or more of ethylene oxide, propylene oxide, and pentane oxide. Among them, ethylene oxide is the simplest cyclic ether, belongs to heterocyclic compounds, and is an important petrochemical product. The epoxy ethane is colorless transparent liquid at low temperature, is colorless gas with ether pungent odor at normal temperature, and is mainly used for preparing other various solvents, diluents, nonionic surfactants, synthetic detergents, antifreeze agents, disinfectants, toughening agents, plasticizers and the like. The water-soluble resin can be synthesized by the hydroxyethylation of the cellulose. It can also be used as fumigant, coating thickener, emulsifier, adhesive, paper sizing agent, etc.
In some embodiments, as shown in fig. 2, step S2, feeding the phosphate ester to the first microchannel reactor via the first metering pump may include: step S21, mixing phosphate and a catalyst in proportion to obtain mixed phosphate; and step S22, the mixed phosphate is pumped to a first microchannel reactor through a first metering pump, and the catalyst is used to accelerate the reaction rate, improve the production capacity, improve the operation conditions, reduce the requirements on equipment and improve the production conditions.
In some embodiments, the catalyst may include any one or more of titanium oxide acetylacetonate, alpha stannous, stannous octoate, C2H5 ONa. Titanium oxide acetylacetonate, alpha stannous, stannous octoate, C 2 H 5 ONa has extremely high catalytic activity and selectivity to the reaction, and can improve the reaction effect.
In some embodiments, the molar ratio of the phosphate, the solid phosphorus pentoxide, the catalyst and the alkylene oxide can be 1:0.51:0.012:0.535-1:0.16:0.022:0.63, and the molar ratio can ensure that the components are fully reacted, thereby improving the reaction effect and reducing the cost.
In some embodiments, the molar ratio of the phosphate, the solid phosphorus pentoxide, the catalyst and the alkylene oxide can be 1:0.55:0.016:0.58, and the molar ratio can ensure that the components are fully reacted, so that the reaction effect is improved and the cost is reduced.
In some embodiments, the pumping flow rate of the second metering pump is 25ml/min-35ml/min, the pumping flow rate of the third metering pump is 10ml/min-20ml/min, and the reaction temperature and the reaction pressure of the microchannel reactor are controlled by controlling the appropriate pumping flow rate, so that the reaction effect is improved.
In some embodiments, the pumping flow rate of the second metering pump is 32ml/min-35ml/min, the pumping flow rate of the third metering pump is 14ml/min-18ml/min, and the reaction temperature and the reaction pressure of the microchannel reactor are controlled by controlling the appropriate pumping flow rate, so that the reaction effect is improved.
In some embodiments, as shown in fig. 3, step S3, reacting solid phosphorus pentoxide and phosphate ester in a first microchannel reactor to obtain a first liquid intermediate material comprising: step S31, preheating solid phosphorus pentoxide and phosphate; and step S32, reacting the preheated solid phosphorus pentoxide and the phosphate in a first microchannel reactor to obtain a first liquid intermediate material. The preheating mode can adopt the jacket oil bath mode for heat the cooling to it, compare in the water bath, the heating temperature upper limit of oil bath is higher, and heating temperature is stable, makes the reactant be heated evenly, uses the activity that the pre-heater can fully improve the reactant, makes the reaction process more abundant, has improved the reaction effect.
In some embodiments, as shown in fig. 4, in step S6, reacting the first liquid intermediate stream with an alkylene oxide in a second microchannel reactor to obtain a second liquid intermediate stream, comprising: step S61, preheating the first liquid intermediate material and the alkylene oxide; and step S62, reacting the preheated first liquid intermediate material with the alkylene oxide in a second microchannel reactor to obtain a second liquid intermediate material. The preheating mode can adopt the jacket oil bath mode for heat the cooling to it, compare in the water bath, the heating temperature upper limit of oil bath is higher, and heating temperature is stable, makes the reactant be heated evenly, uses the activity that the pre-heater can fully improve the reactant, makes the reaction process more abundant, has improved the reaction effect.
In some embodiments, as shown in fig. 5, a method for continuous synthesis of alkyl phosphate esters using a microchannel reactor further comprises: step S81, detecting the pumping pressures of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump to obtain pressure data; and step S82, based on the pressure data, adjusting the pumping flow rates of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump, monitoring the pressure of the reaction process, feeding back to the alarm device in time when the reaction pressure is too high or too low, and controlling and adjusting the pumping flow rates of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump through a manual or automatic control device to enable the reaction pressure to return to normal.
In some embodiments, as shown in fig. 6, a method for continuous synthesis of alkyl phosphate esters using a microchannel reactor further comprises: step S91, detecting the reaction temperature of the first microchannel reactor and the second microchannel reactor to obtain temperature data; and step S92, based on the temperature data, adjusting the pumping flow rates of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump, monitoring the temperature in the reaction process, feeding back to the alarm device in time when the reaction temperature is too high or too low, and controlling and adjusting the pumping flow rates of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump through a manual or automatic control device to enable the reaction temperature to return to normal.
In some embodiments, the reaction temperature is 40-60 ℃ and the reaction time is 10-30min in step S3, and the reaction temperature is 80-120 ℃ and the reaction time is 60-300S in step S6, so that the reaction of the components can be fully performed, and the generation of by-products due to insufficient reaction caused by too low or too high temperature and the waste of reaction time can be avoided.
In some embodiments, the reaction temperature is 45-55 ℃ and the reaction time is 15-25min in step S3, and the reaction temperature is 95-105 ℃ and the reaction time is 120-240S in step S6, so that the reaction of the components can be fully performed at the above reaction temperature and reaction time, and the generation of by-products due to insufficient reaction caused by too low or too high temperature and the waste of reaction time can be avoided.
Based on the same inventive concept, as shown in fig. 7, the present invention also provides an apparatus for continuously synthesizing alkyl phosphate using a microchannel reactor, comprising: the screw conveyor 1 is connected with the first microchannel reactor 5, and is used for conveying the solid phosphorus pentoxide to the first microchannel reactor 5; the first metering pump 3 is connected with the first microchannel reactor 5, and is used for pumping the phosphate to the first microchannel reactor 5; the first microchannel reactor 5 is used for reacting solid phosphorus pentoxide with phosphate to obtain a first liquid intermediate material; the second metering pump 4 is connected with the second microchannel reactor 6, and is used for pumping the first liquid intermediate material to the second microchannel reactor 6; the third metering pump is connected with the second microchannel reactor and is used for pumping the alkylene oxide to the second microchannel reactor 6; the second microchannel reactor 6 is used for reacting the first liquid intermediate material with the alkylene oxide to obtain a second liquid intermediate material; the fourth metering pump is connected with the collecting tank 7 and is used for pumping the second liquid intermediate material to the collecting tank 7; and the collecting tank 7 is used for carrying out reduced pressure rectification on the second liquid intermediate material, and collecting fractions to obtain the alkyl phosphate.
When the device is used, solid phosphorus pentoxide is conveyed to a first microchannel reactor through a screw conveyer, nitrogen purging is carried out on the screw conveyer after feeding through a nitrogen purging port 2, the phenomenon that solid material powder is adhered to the screw conveyer to block the screw conveyer is effectively avoided, meanwhile, phosphate is conveyed to the first microchannel reactor through a first metering pump, the solid phosphorus pentoxide and the phosphate react in the first microchannel reactor to obtain a first liquid intermediate product, the first liquid intermediate product is conveyed to a second microchannel reactor through a second metering pump, alkylene oxide is conveyed to the second microchannel reactor through a third metering pump, the first liquid intermediate product and the alkylene oxide react in the second microchannel reactor to obtain a second liquid intermediate product, and the second liquid intermediate product is conveyed to a collection tank through a fourth metering pump, and carrying out reduced pressure rectification on the second liquid intermediate material, and collecting fractions to obtain a final product, namely the alkyl phosphate. The micro reaction device of the embodiment can realize the addition of solid material powder, and meanwhile, the whole reaction process is divided into two steps to be carried out, so that the whole reaction process is optimized, and the reaction efficiency is improved.
In some embodiments, the first microchannel reactor and the second microchannel reactor are sealed, so that the pressure in the process of synthesizing the alkyl phosphate can be ensured, and the reaction is more complete.
In some embodiments, the apparatus for continuously synthesizing alkyl phosphate using a microchannel reactor further comprises a plurality of pressure sensors, wherein the plurality of pressure sensors are respectively disposed in the first metering pump, the second metering pump, the third metering pump, and the fourth metering pump, and are used for detecting pumping pressures of the first metering pump, the second metering pump, the third metering pump, and the fourth metering pump to obtain pressure data; and adjusting the pumping flow rates of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump based on the pressure data. The temperature of the reaction process is monitored by using the pressure sensor, when the reaction pressure is too high and too low, the pressure sensor can feed back to the alarm device in time, and the pumping flow rates of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump can be controlled and adjusted by a manual or automatic control device.
In some embodiments, an apparatus for continuously synthesizing alkyl phosphate using a microchannel reactor further comprises a plurality of temperature sensors, wherein the plurality of temperature sensors are respectively disposed in the first microchannel reactor and the second microchannel reactor, and are used for detecting reaction temperatures of the first microchannel reactor and the second microchannel reactor to obtain temperature data; and adjusting the pumping flow rates of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump. The temperature sensor is used for monitoring the temperature of the reaction process, when the reaction temperature is too high or too low, the temperature sensor can feed back to the alarm device in time, and the reaction process can be controlled through manual work or an automatic control device.
In some embodiments, an apparatus for continuously synthesizing alkyl phosphate esters using a microchannel reactor further comprises a screening device for screening solid phosphorus pentoxide, wherein fine particulate phosphorus pentoxide passing through the screen of the screening device enters the first microchannel reactor. The reaction degree of solid materials is related to the specific surface area of the solid materials, the larger the specific surface area of solid particles with smaller granularity is, the higher the reaction efficiency is, on the other hand, in the microchannel reaction device, the cross sectional area of a channel is smaller, the solid particles have larger influence on the flow rate and are easy to block, the blocking is avoided for ensuring the efficiency of the reaction process, the solid phosphorus pentoxide needs to be ensured to be in the small enough granularity, the solid phosphorus pentoxide larger than the required granularity on a sieve can be sieved out before the reaction is carried out by arranging a sieving device, the phosphorus pentoxide meeting the required granularity under the sieve enters a first microchannel reactor, the blocking phenomenon of a microchannel is avoided, the solid materials are smoothly reacted by adopting the microchannel reaction device, and then the reaction efficiency is ensured and the first liquid intermediate materials with higher purity and quality are obtained.
In some embodiments, the first microchannel reactor comprises: a first preheating section and a first reaction section; the second microchannel reactor comprises: a second preheating section and a second reaction section; the screw conveyer and the first metering pump are respectively connected with the first preheating section, the first preheating section is connected with the first reaction section, the second metering pump and the third metering pump are respectively connected with the second preheating section, and the second preheating section is connected with the second reaction section. As shown in fig. 8, the microchannel structure may include a straight flow type structure, such as a of fig. 8, and a pulse diameter-variable type structure. The pulse reducing type structure may include a diamond pulse reducing type structure, as shown in b of fig. 8; a heart-shaped pulse reducing structure, as shown in fig. 8 c; and d in figure 8. The preheating mode can adopt and press from both sides cover oil bath mechanism for heat the cooling to it, compare in the water bath, the heating temperature upper limit of oil bath is higher, and heating temperature is stable, makes the reactant be heated evenly, uses the activity that the pre-heater can fully improve the reactant, makes the reaction process more abundant, has improved the reaction effect.
In some embodiments, the first and second preheating stages are a dc configuration; the first reaction section and the second reaction section are of pulse variable-diameter structures, and different micro-channel structures can enhance mass transfer and heat transfer performances, keep the reaction temperature constant, avoid a temperature runaway phenomenon, reduce the generation of by-products, and improve the safety of the reaction process.
The working process of the invention is roughly as follows: conveying solid phosphorus pentoxide to a first microchannel reactor through a screw conveyor, blowing nitrogen through a nitrogen blowing port on the fed screw conveyor to effectively avoid solid powder from adhering to the screw conveyor to block the screw conveyor, simultaneously conveying phosphate to the first microchannel reactor through a first metering pump, reacting the solid phosphorus pentoxide and the phosphate in the first microchannel reactor to obtain a first liquid intermediate product, conveying the first liquid intermediate product to a second microchannel reactor through a second metering pump, conveying alkylene oxide to the second microchannel reactor through a third metering pump, reacting the first liquid intermediate product and the alkylene oxide in the second microchannel reactor to obtain a second liquid intermediate product, conveying the second liquid intermediate product to a collection tank through a fourth metering pump, decompressing and refining the second liquid intermediate product, collecting the fractions to obtain the final product, namely alkyl phosphate. The reaction process is monitored by the temperature sensor and the pressure sensor in the reaction process, when the temperature and the pressure in the reaction process are abnormal, feedback alarm can be carried out, and the reaction process can be controlled by manpower or a control device in time.
In some embodiments, the first preheating section and the second preheating section of the device for continuously synthesizing alkyl phosphate by using the microchannel reactor adopt a direct-current structure, the first reaction section and the second reaction section adopt a rhombic pulse diameter-variable structure, and the heat exchange medium is heat conduction oil. Mixing phosphate and stannous octoate in proportion, controlling the reaction temperature to be 40 ℃ with phosphorus pentoxide after the mixture is reacted for 30min to obtain a first liquid intermediate material, taking ethylene oxide liquid as a raw material B, injecting the raw material B into a reactor through a metering pump at the flow rates of 25ml/min and 10ml/min respectively, controlling the temperature to be 120 ℃ and the reaction time to be 60s, quantitatively collecting reaction liquid, then carrying out reduced pressure distillation, and finally weighing and calculating to obtain the product, namely the yield of the alkyl phosphate, of 98.8%. The alkyl phosphate was analyzed by GC for a purity of 99.4%.
In some embodiments, the first preheating section and the second preheating section of the device for continuously synthesizing alkyl phosphate by using the microchannel reactor adopt a direct-current structure, the first reaction section and the second reaction section adopt a rhombic pulse diameter-variable structure, and the heat exchange medium is heat conduction oil. Mixing phosphate and acetylacetone titanium oxide in proportion, controlling the reaction temperature to be 45 ℃ with phosphorus pentoxide after the mixture is reacted for 25min to obtain a first liquid intermediate material, taking ethylene oxide liquid as a raw material B, injecting the raw material B into a reactor through a metering pump at the flow rates of 35ml/min and 20ml/min respectively, controlling the temperature to be 105 ℃ and the reaction time to be 120s, quantitatively collecting reaction liquid, then carrying out reduced pressure distillation, and finally weighing and calculating to obtain the product, namely the yield of the alkyl phosphate, of 97.1%. The alkyl phosphate was analyzed by GC for a purity of 98.3%.
In some embodiments, the first preheating section and the second preheating section of the device for continuously synthesizing alkyl phosphate by using the microchannel reactor adopt a direct-current structure, the first reaction section and the second reaction section adopt a rhombic pulse diameter-variable structure, and the heat exchange medium is heat conduction oil. Mixing phosphate and alpha stannous according to a certain proportion, controlling the reaction temperature to be 55 ℃ with phosphorus pentoxide, reacting for 15min to obtain a first liquid intermediate material, taking ethylene oxide liquid as a raw material B, injecting the raw material B into a reactor through a metering pump at flow rates of 32ml/min and 14ml/min respectively, controlling the temperature to be 95 ℃ and the reaction time to be 240s, quantitatively collecting reaction liquid, then carrying out reduced pressure distillation, and finally weighing and calculating to obtain the product, namely the yield of the alkyl phosphate, of 95.6%. The alkyl phosphate was analyzed by GC for a purity of 96.8%.
In some embodiments, the first preheating section and the second preheating section of the device for continuously synthesizing alkyl phosphate by using the microchannel reactor adopt a direct-current structure, the first reaction section and the second reaction section adopt a rhombic pulse diameter-variable structure, and the heat exchange medium is heat conduction oil. Mixing phosphate and C2H5ONa in proportion, controlling the reaction temperature to be 60 ℃ with phosphorus pentoxide after the mixture is reacted for 10min to obtain a first liquid intermediate material, taking ethylene oxide liquid as a raw material B, injecting the raw material B into a reactor through a metering pump at the flow rates of 35ml/min and 18ml/min respectively, controlling the temperature to be 80 ℃ and the reaction time to be 300s, quantitatively collecting reaction liquid, then carrying out reduced pressure distillation, and finally weighing and calculating to obtain the product, namely the yield of the alkyl phosphate, of 95.1%. The purity of the alkyl phosphate was 96.1% by GC analysis.
It is to be understood that the term "plurality" as used herein refers to two or more, and other terms are intended to be analogous. "and/or" describes the association relationship of the associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a exists alone, A and B exist simultaneously, and B exists alone. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship. The singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
It will be further understood that the terms "first," "second," and the like are used to describe various information and that such information should not be limited by these terms. These terms are only used to distinguish one type of information from another and do not denote a particular order or importance. Indeed, the terms "first," "second," and the like are fully interchangeable. For example, first information may also be referred to as second information, and similarly, second information may also be referred to as first information, without departing from the scope of the present invention.
It will be further understood that the terms "central," "longitudinal," "lateral," "front," "rear," "upper," "lower," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in an orientation or positional relationship indicated in the drawings for convenience in describing the present embodiment and to simplify the description, but do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation.
It will be further understood that, unless otherwise specified, "connected" includes direct connections between the two without the presence of other elements, as well as indirect connections between the two with the presence of other elements.
It is further to be understood that while operations are depicted in the drawings in a particular order, this is not to be understood as requiring that such operations be performed in the particular order shown or in serial order, or that all illustrated operations be performed, to achieve desirable results. In certain environments, multitasking and parallel processing may be advantageous.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure disclosed herein. This invention is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.
It will be understood that the invention is not limited to the precise arrangements described above and shown in the drawings and that various modifications and changes may be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.

Claims (22)

1. A method for continuously synthesizing alkyl phosphate by using a microchannel reactor is characterized by comprising the following steps:
s1: conveying the solid phosphorus pentoxide to a first microchannel reactor by a screw conveyor;
s2: feeding phosphate to the first microchannel reactor by a first metering pump;
s3: reacting the solid phosphorus pentoxide and the phosphate in the first microchannel reactor to obtain a first liquid intermediate material;
s4: feeding the first liquid intermediate material to a second microchannel reactor through a second metering pump;
s5: sending alkylene oxide to the second microchannel reactor via a third metering pump;
s6: reacting the first liquid intermediate material with the alkylene oxide in the second microchannel reactor to obtain a second liquid intermediate material;
s7: and (4) sending the second liquid to a collecting tank through a fourth metering pump, carrying out reduced pressure rectification, and collecting fractions to obtain the alkyl phosphate.
2. The method for continuously synthesizing alkyl phosphate by using the microchannel reactor as claimed in claim 1, wherein the phosphate comprises any one or more of trimethyl phosphate, triethyl phosphate, tripropyl phosphate, tributyl phosphate and dimethyl methyl phosphate.
3. The method for continuously synthesizing alkyl phosphate by using the microchannel reactor as claimed in claim 1, wherein the alkylene oxide comprises any one or more of ethylene oxide, propylene oxide and pentane oxide.
4. The method of claim 1, wherein the step S2 of feeding the phosphate ester to the first microchannel reactor by the first metering pump comprises:
mixing the phosphate with a catalyst in proportion to obtain mixed phosphate;
pumping the mixed phosphate ester through the first metering pump to the first microchannel reactor.
5. The method for continuously synthesizing alkyl phosphate by using the microchannel reactor as claimed in claim 4, wherein the catalyst comprises titanium oxide acetylacetonate, alpha stannous, stannous octoate, solid pyrophosphoric acid, C 2 H 5 Any one or more of ONa.
6. The method of claim 4, wherein the alkyl phosphate is continuously synthesized by using a microchannel reactor, and the method comprises the following steps: the molar ratio of the phosphate, the solid phosphorus pentoxide, the catalyst and the alkylene oxide is 1: 0.51-0.16: 0.012-0.22: 0.535-0.63.
7. The method of claim 6, wherein the alkyl phosphate is continuously synthesized by using a microchannel reactor, and the method comprises the following steps: the molar ratio of the phosphate, the solid phosphorus pentoxide, the catalyst and the alkylene oxide is 1:0.55:0.016: 0.58.
8. The method for continuously synthesizing alkyl phosphate by using the microchannel reactor as claimed in claim 1, wherein the pumping flow rate of the second metering pump is 25ml/min to 35ml/min, and the pumping flow rate of the third metering pump is 10ml/min to 20 ml/min.
9. The method for continuously synthesizing alkyl phosphate by using the microchannel reactor as claimed in claim 1, wherein the pumping flow rate of the second metering pump is 32ml/min to 35ml/min, and the pumping flow rate of the third metering pump is 14ml/min to 18 ml/min.
10. The method of claim 1, wherein the step S3 of reacting the solid phosphorus pentoxide and the phosphate ester in the first microchannel reactor to obtain a first liquid intermediate material comprises:
preheating the solid phosphorus pentoxide and the phosphate ester;
and reacting the preheated solid phosphorus pentoxide and the phosphate in the first microchannel reactor to obtain a first liquid intermediate material.
11. The method of claim 1, wherein the step S6 of reacting the first liquid intermediate material and the alkylene oxide in the second microchannel reactor to obtain a second liquid intermediate material comprises:
preheating the first liquid intermediate stream and the alkylene oxide;
and reacting the preheated first liquid intermediate material and the alkylene oxide in the second microchannel reactor to obtain a second liquid intermediate material.
12. The method of claim 1, further comprising the step of:
detecting pumping pressures of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump to obtain pressure data;
and adjusting the pumping flow rates of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump based on the pressure data.
13. The method of claim 1, further comprising the step of:
detecting the reaction temperature of the first microchannel reactor and the second microchannel reactor to obtain temperature data;
adjusting pumping flow rates of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump based on the temperature data.
14. The method of claim 9, wherein the reaction temperature is 40-60 ℃ and the reaction time is 10-30min in step S3, and the reaction temperature is 80-120 ℃ and the reaction time is 60-300S in step S6.
15. The method as claimed in claim 10, wherein the reaction temperature is 45-55 ℃ and the reaction time is 15-25min in step S3, and the reaction temperature is 95-105 ℃ and the reaction time is 120-240S in step S6.
16. An apparatus for continuously synthesizing alkyl phosphate using a microchannel reactor, comprising:
the screw conveyer is connected with the first micro-channel reactor and is used for conveying the solid phosphorus pentoxide to the first micro-channel reactor;
the first metering pump is connected with the first microchannel reactor and is used for pumping the phosphate to the first microchannel reactor;
a first microchannel reactor for reacting the solid phosphorus pentoxide with the phosphate ester to obtain a first liquid intermediate material;
the second metering pump is connected with the second microchannel reactor and is used for pumping the first liquid intermediate material to the second microchannel reactor;
a third metering pump connected to the second microchannel reactor for pumping alkylene oxide to the second microchannel reactor;
a second microchannel reactor for reacting the first liquid intermediate material with the alkylene oxide to obtain a second liquid intermediate material;
the fourth metering pump is connected with the collecting tank and is used for pumping the second liquid intermediate material to the collecting tank; and the collecting tank is used for carrying out reduced pressure rectification on the second liquid intermediate material, and collecting fractions to obtain the alkyl phosphate.
17. The apparatus of claim 16, wherein the first microchannel reactor and the second microchannel reactor are sealed.
18. The apparatus according to claim 17, further comprising:
the pressure sensors are respectively arranged on the first metering pump, the second metering pump, the third metering pump and the fourth metering pump and are used for detecting the pumping pressures of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump to obtain pressure data; adjusting pumping flow rates of the first, second, third, and fourth metering pumps based on the pressure data.
19. The apparatus according to claim 17, further comprising:
the temperature sensors are respectively arranged on the first microchannel reactor and the second microchannel reactor and are used for detecting the reaction temperatures of the first microchannel reactor and the second microchannel reactor to obtain temperature data; and adjusting the pumping flow rates of the first metering pump, the second metering pump, the third metering pump and the fourth metering pump.
20. The apparatus according to claim 16, further comprising:
and the screening device is used for screening the solid phosphorus pentoxide, wherein the undersize fine-particle phosphorus pentoxide which passes through the screening device enters the first microchannel reactor.
21. The apparatus for continuously synthesizing alkyl phosphate using a microchannel reactor as set forth in any one of claims 16 to 20,
the first microchannel reactor comprises: a first preheating section and a first reaction section;
the second microchannel reactor comprises: a second preheating section and a second reaction section;
the spiral conveyor and the first metering pump are respectively connected with the first preheating section, the first preheating section is connected with the first reaction section, the second metering pump and the third metering pump are respectively connected with the second preheating section, and the second preheating section is connected with the second reaction section.
22. The apparatus of claim 21, wherein the first preheating section and the second preheating section have a straight-flow configuration; the first reaction section and the second reaction section are of pulse variable-diameter structures.
CN202210570634.5A 2022-05-24 2022-05-24 Method and device for continuously synthesizing alkyl phosphate by using microchannel reactor Pending CN114832752A (en)

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CN207756114U (en) * 2017-12-29 2018-08-24 山东金德新材料有限公司 The continuous powder injection device of high-precision for microreactor
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CN107903440A (en) * 2017-11-29 2018-04-13 云南云天化以化磷业研究技术有限公司 A kind of Halogen alkyl phosphoric acid ester oligomer organic fire-retardant and preparation method thereof
CN207756114U (en) * 2017-12-29 2018-08-24 山东金德新材料有限公司 The continuous powder injection device of high-precision for microreactor
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