CN111905668B - Reaction device and application thereof in continuous preparation of vegetable oil polyalcohol - Google Patents
Reaction device and application thereof in continuous preparation of vegetable oil polyalcohol Download PDFInfo
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- CN111905668B CN111905668B CN202010920442.3A CN202010920442A CN111905668B CN 111905668 B CN111905668 B CN 111905668B CN 202010920442 A CN202010920442 A CN 202010920442A CN 111905668 B CN111905668 B CN 111905668B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/245—Stationary reactors without moving elements inside placed in series
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
- C07C67/31—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by introduction of functional groups containing oxygen only in singly bound form
Abstract
The invention discloses a reaction device and application thereof in continuously preparing vegetable oil polyalcohol, wherein the reaction device is formed by sequentially connecting a plurality of reaction kettles in series; wherein a jacket is arranged outside the kettle body of the reaction kettle; the reactor body of the reaction kettle is internally provided with a baffle plate, a plurality of arc baffle plates are arranged between every two adjacent layers of baffle plates, and the arc baffle plates are fixed on the baffle plates at two sides. The preparation process is easy to operate and control, and the reaction temperature of the multistage reaction kettle is compartmentalized, so that the side reaction is effectively weakened. The baffle design in the production equipment has effectually solved the viscosity problem in the enlarged production of continuous preparation vegetable oil polyalcohol, has produced better mixed effect, and simultaneously, the effectual pressure differential problem of having solved of baffle design through the last manometer of reation kettle demonstration, can be with the pressure differential control of reation kettle at different levels within 1 atmosphere, and the performance requirement to the pump is low.
Description
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to a reaction device and application thereof in continuous preparation of vegetable oil polyol.
Background
With the increase of petroleum consumption, the storage of petrochemical resources is increasingly reduced, the price of petrochemical products is continuously increased, the production of materials and fuels from renewable resources is more and more important, and the use of renewable resources as raw materials of chemical products is concerned by people. The vegetable oil polyalcohol is a substitute of petroleum-based polyalcohol, and has outstanding environmental protection value. According to the analysis data of the biosphere, compared with petroleum-based polyol, the total energy consumption of the vegetable oil polyol is reduced by 23%, the non-renewable resource consumption is reduced by 61%, and the emission of greenhouse gases to the atmosphere is reduced by 36%. The vegetable oil polyalcohol has wide raw material sources, and the vegetable oil comprises edible oil such as peanut oil, rapeseed oil, soybean oil, castor oil, olive oil, palm oil and the like, and non-edible oil such as jatropha curcas oil, pistacia chinensis bunge oil and the like.
The vegetable oil polyalcohol is mainly applied to the field of polyurethane, and the prepared vegetable oil-based polyurethane material completely meets the requirement of environmental protection; and because of the hydrophobicity of the main component fatty glyceride of the vegetable oil, the vegetable oil-based polyurethane material has good physical and chemical properties, particularly better hydrolysis resistance and thermal stability. Thus, vegetable oil polyols and their polyurethane materials have been rapidly developed.
The vegetable oil mainly comprises fatty glyceride, and most vegetable oils contain 14-22 carbon chain fatty acids, and each fatty acid has 0-3 unsaturated double bonds. In addition to castor oil, vegetable oils must be hydroxyl functionalized to provide polyols for the synthesis of polyurethane materials. The vegetable oil polyol is mainly divided into the following 5 types according to different synthetic methods: an alcoholysis method comprises the following steps: the vegetable oil is alcoholyzed by using ester group in the vegetable oil and micromolecular alcohol with multiple functionality, and hydroxyl is introduced on a molecular chain. ② epoxy ring opening method: the carbon-carbon double bond of the vegetable oil is epoxidated by Prileshajev, and then the epoxy group is opened by a functional monomer to introduce hydroxyl. ③ ozone oxidation method: double bonds in the vegetable oil are oxidized by utilizing the strong oxidizing property of ozone, so that the double bonds are broken to form primary hydroxyl groups or carboxylic acid groups, and then the carboxylic acid groups are subjected to esterification and other reactions to prepare the vegetable oil polyol. (iv) hydroformylation process: double bonds of the vegetable oil are utilized, a noble metal catalyst is adopted to react with hydrogen and carbon monoxide under certain pressure to generate aldehyde, and then hydrogenation is carried out to convert the aldehyde into hydroxyl. Alkoxylation: the production method of the similar petroleum-based polyol is to prepare the vegetable oil polyol by directly mixing vegetable oil and small molecular alcohol as a starting agent (or directly using vegetable oil containing hydroxyl as the starting agent) and performing alkoxylation. The method for preparing the vegetable oil polyol by the epoxy ring-opening method is low in cost and is a currently accepted method which is most likely to realize industrialization in the polyurethane industry.
Under the catalysis of sulfuric acid or fluoboric acid, the vegetable oil polyol is prepared by ring opening of water, alcohol amine, carboxylic acid and the like. Wherein, the vegetable oil polyalcohol with the structure of ortho-dihydroxy can be generated by the ring opening of the epoxidized vegetable oil through water. CN1837180A and CN101139252A respectively disclose "a bio-based polyol prepared by using rapeseed oil" and "a bio-based polyol prepared by using jatropha curcas oil", wherein the vegetable oil polyol is prepared by using the rapeseed oil and the jatropha curcas oil as main raw materials and carrying out three-step reactions of alcoholysis/epoxidation/ring opening. CN1837181A and CN101108803A disclose "a bio-based polyol prepared from rapeseed oil" and "a bio-based polyol prepared from jatropha curcas oil", which are respectively prepared from rapeseed oil and jatropha curcas oil as main raw materials through three steps of epoxidation/ring opening/alcoholysis to obtain vegetable oil polyol. CN1907944A discloses a bio-based polyol prepared by epoxy rapeseed oil, which directly takes the epoxy rapeseed oil as a main raw material to prepare vegetable oil polyol through two steps of ring opening/alcoholysis reaction. CN101906016A discloses a rubber seed oil polyol and a preparation method thereof, which takes rubber seed oil as a main raw material and prepares the vegetable oil polyol through two-step reaction of epoxidation/ring opening. CN101659627A discloses a high hydroxyl value bio-based polyol prepared by one-step reaction of epoxidized vegetable oil, which is prepared by the epoxy group ring-opening reaction and ester amidation reaction of the epoxidized vegetable oil and glycol amine. CN101747184A and CN101230020A disclose respectively a method for preparing polyol from soybean oil by one-step method and a method for synthesizing macromonomer for polymer polyol by vegetable oil and application thereof, and vegetable oil polyol is prepared by one-step method by reacting epoxidation and ring opening under acidic condition.
The vegetable oil polyol prepared by the above patents is mainly based on epoxy group open loop and is synthesized by an intermittent reaction kettle, and the following disadvantages exist: the reaction time is long; secondly, the energy consumption is higher; the equipment and the automatic control level are low; and fourthly, the quality of the product is low due to the inevitable side reaction (the hydroxyl value of the product is low and the viscosity is large due to the crosslinking side reaction).
Because vegetable oil has lipophilicity, large molecular weight and higher viscosity than common reagents, ring-opening reagents cannot be mixed with vegetable oil molecules, liquid-liquid two-phase reaction mass transfer efficiency is low, and when an intermittent mode is adopted, the rotating speed of a stirring paddle is not high, the reaction time is long, a plurality of side reactions are brought, and the quality is reduced. Aiming at the derivatization reaction of vegetable oil, the micro-flow field reaction technology can enhance the mass transfer process, reduce the reaction time and improve the product quality by a certain promotion effect through a scale effect, the development of vegetable oil polyol by adopting the micro-flow field reaction technology has been applied to a certain extent at present, however, most of vegetable oil derivatization systems are successful only in a laboratory, once entering a pilot scale amplification stage, process simulation and calculation are carried out, a pipeline often needs hundreds of meters or more to reach a pilot scale level after the flow velocity is amplified, at the moment, the system bears a larger pressure difference and puts a very high requirement on a feed pump, and as the local pressure of the system is larger, the situations of liquid leakage and inaccurate pump feeding or difficult to maintain for a long time occur, the process of pilot scale amplification and production is greatly influenced, at present, the amplification can be realized only by adopting a flow velocity reduction mode, however, since the decrease in the flow rate leads to a decrease in the mass transfer efficiency, which may result in longer or longer residence times for the tubing and cross-linking side reactions, it is difficult to achieve laboratory levels simply by scaling up the microfluidic laboratory technology. Based on the above, the calculation simulation of various reaction systems is carried out, the material properties of the vegetable oil and the ring-opening reagent are considered, the relation between the scale effect and the mass transfer is considered, the influence of the linear flow velocity and the volume flow velocity is considered, the study of the main reaction and the side reaction kinetics is combined, the experiment-level mass transfer effect is found to be realized, the length of the pipeline is 200-1000m under the condition that the pipe diameter is 0.4-1 cm and the pipeline is internally provided with components for assistance, at the moment, the pressure difference of the pipeline is possibly 80-300atm, if the material is conveyed by a pump, the system requirement is difficult to meet, and through the attempt, even if the pump with the working pressure of 100atm is used, the long-time conveying can not be met, the feeding error and even damage can occur with a large probability of working for several hours, therefore, the reaction systems, the equipment matching and the reaction effect are difficult to be coordinated, it is necessary to develop new process or equipment, improve the existing amplification process, maintain the continuous flow process, consider the coordination of the micro-reaction characteristic and the equipment working state, and realize the stable and effective operation of pilot amplification in the derivatization process of the vegetable oil.
Taking CN103288642B 'a method for preparing vegetable oil polyalcohol by using a continuous method' as an example, the method discloses that epoxy vegetable oil is processed by H2And O, performing ring opening in one step to prepare the vegetable oil polyol. The method develops the vegetable oil polyol with higher viscosity, adopts the microchannel modular reaction device to rapidly prepare the product, has continuous operation, easy operation and control of the preparation process, short reaction time, small pollution, low energy consumption, weakened side reaction and larger controllable hydroxyl value range of the product. First, this method allows for small runs in a microreactor device, but presents the problems described above when scaled up. When utilizing traditional equipment to enlarge, because product viscosity is big, in order to reach better mixed effect, need improve the velocity of flow and strengthen mass transfer efficiency, but because pressure differential is great, must only reduce the velocity of flow so that the effective transport of pump, still can produce the pressure differential of 20 ~ 40atm, the pump is difficult to maintain under long-time operating condition, when carrying out 2 ~ 4L enlargies, must use the pump of Germany import, otherwise can lead to the pump to produce trouble and measure inaccurate condition, to a great extent has restricted the application. Secondly, in the scale-up experiment, the pump needs to be calibrated many times, the flow rate is difficult to maintain, if the reaction process needs to be stabilized, the flow rate can only be reduced again, the mass transfer efficiency is reduced, and the time is prolonged, so that the increase of the by-products is caused.
Based on the problems, the novel equipment for continuously preparing the vegetable oil polyol not only keeps the characteristics of the micro-reaction scale effect, but also weakens the strength of a reaction system through process design, effectively reduces the system pressure and improves the stability of the reaction system on the basis of calculation simulation and verification of a large amount of experimental data. Aiming at a vegetable oil derivatization system of high-viscosity multiphase liquid-liquid reaction, the novel equipment of a multi-stage reaction kettle with a specific structure design is adopted in the amplification process, the pressure difference of each reaction kettle can be controlled below 1atm, meanwhile, the temperature can be controlled in an interval mode, side reactions are effectively weakened, high temperature sections are reduced, crosslinking is reduced, the effective conversion of functional group epoxy groups to hydroxyl groups is facilitated, and high-viscosity products caused by crosslinking side reactions are avoided. The multistage reaction kettle is used for amplification, the conversion of the epoxy group is almost completely realized, and the reaction effect is equivalent to that of a small test in the patent CN 103288642B. Simultaneously, compare with the traditional experiment reation kettle that enlargies, the effectual pressure differential problem of having solved of baffle design has low to the performance requirement of pump.
Disclosure of Invention
The invention aims to solve the technical problem of providing a reaction device for continuously preparing vegetable oil polyol aiming at the problems of large viscosity, low product quality and high requirement on the performance of a domestic pump in the process of continuously preparing vegetable oil polyol in the prior art.
The invention idea is as follows: the method is characterized in that the method comprises a step of amplifying the methods disclosed in the patent CN103288642B, namely a method for preparing vegetable oil polyalcohol by a continuous method, and the like, because the hydroxyl value is high, cross-linking is easily generated, so that the viscosity is high, and only in order to better improve the mass transfer and heat transfer efficiency, oil and water phases need to be well mixed, a partition plate is arranged in a reaction kettle, an arc-shaped baffle plate is arranged on each layer of partition plate, reaction liquid is ejected after impacting the baffle plate, and flows out from a gap between the baffle plates for next impact, so that the reaction liquid is mixed, the mixing effect is better than that of the traditional amplification experiment size, the pressure difference generated in the reaction kettle is small, and the performance requirement on a plunger pump is not high. In addition, because severe crosslinking is easy to occur in the amplification process, the reaction temperature of each stage of reaction kettle of the multistage reaction kettle is subjected to regional temperature control, the number of reaction kettles in a high-temperature section is reduced, according to the reaction mechanism, the reaction rate is high in the initial stage of the reaction, the reaction is carried out at a lower temperature, the reaction is carried out at a higher temperature in the later stage, the high-temperature section is reduced, and the occurrence of side reactions is effectively inhibited. The reaction time in the multi-stage reaction kettle is longer than that in the microreactor, if the temperature is not controlled, problems can be caused, and the reaction effect can be almost the same as that of a small experiment by controlling the temperature and reducing a high-temperature section.
The invention also aims to solve the technical problem of providing the application of the reaction device in preparation of vegetable oil polyol.
In order to solve the first technical problem, the invention discloses a reaction device which is formed by sequentially connecting a plurality of reaction kettles in series; wherein a jacket 2 is arranged outside the kettle body 1 of the reaction kettle; the reaction kettle is characterized in that a partition plate 3 is arranged inside a kettle body 1 of the reaction kettle, a plurality of arc baffles 4 are arranged between every two adjacent partition plates 3, and the arc baffles 4 are fixed on the partition plates 3 on two sides.
Preferably, the reaction device is formed by sequentially connecting 4-10 reaction kettles in series.
Wherein, the top of the kettle body 1 is respectively provided with a thermometer interface 5, a material inlet 8 and a pressure gauge interface 7; a material outlet 6 is formed at the bottom of the kettle body 1; the upper part of the jacket side wall is provided with a hot coal outlet 9, the lower part of the jacket side wall is provided with a heating medium inlet 10, and the bottom of the jacket is provided with an evacuation port 11.
Wherein, the reactor body 1 of the reaction kettle is internally provided with 5 layers of clapboards/0.5L, and the distance between every two layers of clapboards is 2 cm.
Preferably, the central angle of the circular arc baffle 4 is 90 degrees, the radius is 1cm, and the thickness is 3 mm.
Preferably, the directions of the arc baffles adjacent up and down are opposite; wherein, the convex side of the baffle is the same as the water flow direction.
Preferably, the reaction kettle is a glass reaction kettle.
The reaction device further comprises a pump and a mixer, the two pumps are connected with an inlet of the mixer in a parallel mode, an outlet of the mixer is connected to a material inlet 8 of the first reaction kettle, a material outlet 6 of the first reaction kettle is connected with a material inlet 8 of the second reaction kettle, and the second reaction kettle to the tenth reaction kettle are sequentially connected according to the method. After the reaction is stopped, the reaction kettle is idle, the heat conduction oil or water in the jacket layer can be discharged out through the evacuation port 11, and the evacuation port 11 is in a closed state in the reaction process.
Wherein, the pump is a plunger pump in south pump industry, the model is JX35/12.0, and the power is 0.75 KW.
In order to solve the second technical problem, the invention discloses an application of the reaction device in the continuous preparation of the vegetable oil polyol, wherein the vegetable oil contains unsaturated carbon-carbon double bonds (figure 1), the double bonds can be subjected to Prileshajev epoxidation reaction to prepare the epoxy vegetable oil, and the epoxy vegetable oil can be subjected to ring opening by water under the catalysis of sulfuric acid or fluoboric acid to generate the vegetable oil polyol with an o-dihydroxy structure (figure 2).
Wherein, the application comprises the following steps: the mixer is gone into respectively with the catalyst aqueous solution concurrent pump to epoxy vegetable oil solution, carry out the first reaction in carrying out first reation kettle from first reation kettle's material import (8) after mixing again, carry out the second reaction in carrying out second reation kettle from first reation kettle's material export (6) through second reation kettle's material import (8) again, react in each grade of reation kettle in proper order, after the reaction in last one-level reation kettle, the reaction liquid flows from last one-level reation kettle's material export (6), collect the effluent liquid, thereby realize that the material can be in succession through multistage reation kettle, and its different temperature interval of simultaneous control, realize serialization, high-efficient production.
Preferably, the number of stages of the reaction kettle is 6-10 stages, and the volume of each reaction kettle is 500 mL.
Wherein the epoxy vegetable oil is any one or combination of more of epoxy olive oil, epoxy peanut oil, epoxy rapeseed oil, epoxy cottonseed oil, epoxy soybean oil, epoxy coconut oil, epoxy palm oil, epoxy sesame oil, epoxy sunflower oil, epoxy linseed oil, epoxy castor oil, epoxy tung oil, epoxy safflower oil, epoxy rice bran oil, epoxy corn oil and epoxy tea oil.
The solvent of the epoxy vegetable oil solution is any one or combination of tetrahydrofuran, pyridine, acetone and methyl isobutyl ketone, and the volume ratio of the epoxy vegetable oil to the solvent is 1: 1.5-8, preferably 1: 2-6.
Wherein the volume ratio of the catalyst to water in the catalyst aqueous solution is 1: 15-40, preferably 1: 18-30; the catalyst is 98 wt% of concentrated sulfuric acid or 40 wt% of fluoboric acid.
The amount of the epoxy vegetable oil solution and the catalyst aqueous solution is controlled, so that the volume ratio of the epoxy vegetable oil to the catalyst is 1: 10-20, preferably 1: 10-16.
Wherein the reaction is carried out under normal pressure, the total reaction time is 10-40 min, and the reaction temperature is 30-100 ℃; preferably, the temperature of the latter reaction kettle is more than or equal to that of the former reaction kettle, and the temperature interval is less than or equal to 10 ℃.
Preferably, after the reaction is completed, the reaction solution is allowed to stand for liquid separation, the aqueous phase is recovered, and the oil phase is Na2CO3And washing the aqueous solution to be neutral, and then carrying out liquid separation and rotary evaporation to obtain the vegetable oil polyalcohol.
Wherein, the Na is2CO3Na in aqueous solution2CO3The mass percentage concentration of (B) is 5 wt%.
Has the advantages that: compared with the prior art, the invention has the following advantages:
in the invention, during the amplification process of the 'method for preparing vegetable oil polyalcohol by using a continuous method' disclosed by CN103288642B, the preparation process is easy to operate and control, and the reaction temperature of a multistage reaction kettle is compartmentalized, so that the side reaction is effectively weakened. The baffle design in the production equipment has effectually solved the viscosity problem in the enlarged production of continuous preparation vegetable oil polyalcohol, has produced better mixed effect, and simultaneously, the effectual pressure differential problem of having solved of baffle design through the last manometer of reation kettle demonstration, can be with the pressure differential control of reation kettle at different levels within 1 atmosphere, and the performance requirement to the pump is low.
Drawings
The foregoing and/or other advantages of the invention will become more apparent from the following detailed description of the invention when taken in conjunction with the accompanying drawings.
FIG. 1 shows the chemical structure of vegetable oil.
FIG. 2 is a schematic of the synthesis of vegetable oil polyols.
FIG. 3 is a front view of the reaction vessel.
FIG. 4 is a top view of a reaction vessel.
FIG. 5 is a diagram of baffle dimensions for a reaction vessel.
Fig. 6 is a schematic view of the direction of water flow.
Detailed Description
The invention will be better understood from the following examples. However, those skilled in the art will readily appreciate that the description of the embodiments is only for illustrating the present invention and should not be taken as limiting the invention as detailed in the claims.
Example 1: reaction device
A reaction device is formed by sequentially connecting 4-10 glass reaction kettles in series; the volume of the kettle body of each glass reaction kettle is 500 mL; as shown in fig. 3, a jacket 2 is arranged outside a kettle body 1 of the reaction kettle; the reaction kettle is characterized in that a partition plate 3 is arranged inside a kettle body 1 of the reaction kettle, a plurality of arc baffles 4 are arranged between every two adjacent partition plates 3, and the arc baffles 4 are fixed on the partition plates 3 at the two sides; two sides of the reaction kettle body 1 are provided with hangers.
Wherein, the top of the kettle body 1 is respectively provided with a thermometer interface 5, a material inlet 8 and a pressure gauge interface 7; a material outlet 6 is formed at the bottom of the kettle body 1; the upper part of the jacket side wall is provided with a hot coal outlet 9, the lower part of the jacket side wall is provided with a heating medium inlet 10, and the bottom of the jacket is provided with an evacuation port 11.
Wherein, the reactor body 1 of the reaction kettle is internally provided with 5 layers of clapboards/0.5L, and the distance between every two layers of clapboards is 2 cm.
As shown in fig. 3 to 5, the partition plate 3 is a D-shaped circle, the diameter of the partition plate 3 is 76mm, and the distance between the D-shaped end and the circle center is 26 mm; the partition plate 3 is sequentially provided with 5 rows of arc baffles 4 by taking the circle center as the center, the first row, the third row and the fifth row are respectively provided with three arc baffles, and the second row and the fourth row are provided with two arc baffles; in the second, third and fourth rows, the front-back distance of each smooth baffle 4 is 15mm, and in the first and fifth rows, the front-back distance of each smooth baffle 4 is 7.5 mm; the central angle of the arc baffle 4 is 90 degrees, the radius is 1cm, and the thickness is 3 mm.
Wherein the directions of the upper and lower adjacent arc baffles are opposite; wherein, as shown in fig. 6, the protruding side of the baffle is the same as the water flow direction.
Wherein, the reaction kettle is a glass reaction kettle.
The reaction device further comprises a pump and a mixer, the two pumps are connected with an inlet of the mixer in a parallel mode, an outlet of the mixer is connected to 8 of the first reaction kettle, 6 of the first reaction kettle is connected with 8 of the second reaction kettle, and the second reaction kettle to the tenth reaction kettle are sequentially connected according to the method.
Wherein, the pump is a plunger pump in south pump industry, the model is JX35/12.0, and the power is 0.75 KW.
The multi-stage reaction vessels used in the following examples are all the reaction devices of the present example, and the difference is only in the stage number of the reaction vessels.
Example 2:
dissolving 22.0L of epoxy olive oil in 66.0L of tetrahydrofuran to prepare component A, dissolving 1.4L of sulfuric acid in 26.4L of water to prepare component B, simultaneously pumping into an 8-stage series glass reaction kettle, wherein the reaction temperature of the kettles 1, 2 and 3 is 40 ℃, the reaction temperature of the kettles 4, 5, 6 and 7 is 45 ℃, the reaction temperature of the kettle 8 is 50 ℃, the sample injection rates of A, B components are 102.0mL/min and 32.8mL/min respectively, the reaction time is 30min, standing and separating the reaction products, recovering the water phase, and using 5 wt% of Na as an oil phase2CO3Washing the aqueous solution to be neutral, separating the solution, and performing rotary evaporation to obtain the olive oil polyalcohol with a hydroxyl value of 222mg KOH/g and a viscosity of 5440mPa & s.
Example 3:
dissolving 22.0L of epoxy peanut oil in 110.0L of tetrahydrofuran to prepare component A, dissolving 2.2L of fluoroboric acid in 48.4L of water to prepare component B, simultaneously pumping into a 6-stage series glass reaction kettle, wherein the reaction temperature of a kettle 1 is 65 ℃, the reaction temperatures of kettles 2 and 3 are 70 ℃, the reaction temperatures of kettles 4 and 5 are 75 ℃, the reaction temperature of a kettle 6 is 80 ℃, the sample injection rates of A, B components are 143.1mL/min and 56.8mL/min respectively, the reaction time is 15min, standing and separating the reaction products, recovering the water phase, and using 5 wt% Na as the oil phase2CO3And (3) washing the aqueous solution to be neutral, and then carrying out liquid separation and rotary evaporation to obtain the peanut oil polyol, wherein the hydroxyl value of the peanut oil polyol is 265mg KOH/g, and the viscosity of the peanut oil polyol is 5710mPa & s.
Example 4:
dissolving 22.0L epoxy rapeseed oil in 77.0L tetrahydrofuran to obtain component A, and adding 2.2L sulfuric acidDissolving in 66.0L water to prepare component B, pumping into 6-stage series glass reaction kettle at the same time, wherein the reaction temperature of kettle 1 is 55 deg.C, the reaction temperature of kettles 2 and 3 is 60 deg.C, the reaction temperature of kettles 4 and 5 is 65 deg.C, the reaction temperature of kettle 6 is 70 deg.C, the sample injection rate of A, B component is 149.1mL/min and 100.9mL/min, the reaction time is 12min, standing and separating the reaction product, recovering water phase, and using 5 wt% Na as oil phase2CO3And washing the aqueous solution to be neutral, and then carrying out liquid separation and rotary evaporation to obtain the rapeseed oil polyalcohol, wherein the hydroxyl value of the rapeseed oil polyalcohol is 222mg KOH/g, and the viscosity of the rapeseed oil polyalcohol is 5510mPa & s.
Example 5:
dissolving 22.0L epoxy cottonseed oil in 44.0L tetrahydrofuran to prepare component A, dissolving 1.5L sulfuric acid in 36.4L water to prepare component B, simultaneously pumping into a 6-stage series glass reaction kettle, wherein the reaction temperature of the kettle 1 is 30 ℃, the reaction temperatures of the kettles 2, 3 and 4 are 35 ℃, the reaction temperatures of the kettles 5 and 6 are 40 ℃, the sample injection rates of A, B components are 127.2mL/min and 72.7mL/min respectively, the reaction time is 15min, separating and standing the reaction products, recovering the water phase, using 5% Na as an oil phase2CO3Washing the aqueous solution to be neutral, separating liquid, and performing rotary evaporation to obtain the cottonseed oil polyol, wherein the hydroxyl value of the cottonseed oil polyol is 232mg KOH/g, and the viscosity of the cottonseed oil polyol is 5590mPa & s.
Example 6:
dissolving 22.0L of epoxy soybean oil in 88.0L of tetrahydrofuran to prepare component A, dissolving 1.8L of fluoroboric acid in 33.8L of water to prepare component B, simultaneously pumping into a 6-stage series glass reaction kettle, wherein the reaction temperature of the kettle 1 is 70 ℃, the reaction temperatures of the kettles 2, 3 and 4 are 80 ℃, the reaction temperature of the kettle 5 is 90 ℃, the reaction temperature of the kettle 6 is 100 ℃, the sample injection rates of A, B components are 151.5mL/min and 48.7mL/min respectively, the reaction time is 15min, standing and separating the reaction products, recovering the water phase, and using 5 wt% of Na as an oil phase2CO3Washing the aqueous solution to be neutral, and then carrying out liquid separation and rotary steaming to obtain the soybean oil polyol, wherein the hydroxyl value of the soybean oil polyol is 356mg KOH/g, and the viscosity of the soybean oil polyol is 7730mPa & s.
Example 7:
dissolving 22.0L epoxy coconut oil in 66.0L tetrahydrofuran to prepare component A, dissolving 2.0L fluoroboric acid in 42.2L water to prepare component B, pumping into 7-stage series glass reaction kettle, and keeping the reaction temperature of kettle 1 and kettle 240 ℃, the reaction temperature of the kettles 3, 4 and 5 is 45 ℃, the reaction temperature of the kettles 6 and 7 is 50 ℃, the sample injection rates of the A, B components are respectively 105.0mL/min and 54.1mL/min, the reaction time is 22min, the reaction product is kept stand for liquid separation, the water phase is recovered, the oil phase is prepared by 5 wt% of Na2CO3Washing the coconut oil polyol with the aqueous solution to be neutral, and then carrying out liquid separation and rotary evaporation to obtain the coconut oil polyol, wherein the hydroxyl value of the coconut oil polyol is 250mg KOH/g, and the viscosity of the coconut oil polyol is 6100mPa & s.
Example 8:
dissolving 22.0L epoxy sesame oil in 44.0L tetrahydrofuran to prepare component A, dissolving 1.4L sulfuric acid in 28.0L water to prepare component B, simultaneously pumping into a 7-stage series glass reaction kettle, wherein the reaction temperature of the kettle 1 is 65 ℃, the reaction temperatures of the kettles 2, 3 and 4 are 70 ℃, the reaction temperatures of the kettles 5 and 6 are 75 ℃, the reaction temperature of the kettle 7 is 80 ℃, the sample injection rates of A, B components are 244.9mL/min and 105.1mL/min respectively, the reaction time is 10min, standing and separating the reaction products, recovering the water phase, and using 5 wt% Na as the oil phase2CO3Washing the sesame oil polyol with the aqueous solution to be neutral, and then carrying out liquid separation and rotary steaming to obtain the sesame oil polyol, wherein the hydroxyl value of the sesame oil polyol is 242mg KOH/g, and the viscosity of the sesame oil polyol is 5720mPa & s.
Example 9:
dissolving 22.0L of epoxy sunflower seed oil in 66.0L of tetrahydrofuran to prepare component A, dissolving 1.8L of fluoroboric acid in 32.6L of water to prepare component B, simultaneously pumping into a 6-stage series glass reaction kettle, wherein the reaction temperature of the kettle 1 is 60 ℃, the reaction temperatures of the kettles 2, 3 and 4 are 65 ℃, the reaction temperatures of the kettles 5 and 6 are 70 ℃, the sample injection rates of A, B are 146.1mL/min and 54.1mL/min respectively, the reaction time is 15min, standing and separating the reaction products, recovering the water phase, and using 5 wt% of Na as an oil phase2CO3Washing the aqueous solution to be neutral, separating liquid, and performing rotary steaming to obtain the sunflower seed oil polyalcohol with a hydroxyl value of 343mg KOH/g and a viscosity of 7520mPa & s.
Example 10:
dissolving 22.0L epoxy linseed oil in 132.0L tetrahydrofuran to prepare component A, dissolving 1.9L fluoroboric acid in 38.0L water to prepare component B, and pumping into 6-stage series glass reaction kettle, wherein the reaction temperature of kettle 1 is 75 deg.C, the reaction temperatures of kettles 2 and 3 are 80 deg.C, the reaction temperatures of kettles 4 and 5 are 85 deg.C, the reaction temperature of kettle 6 is 90 deg.C, and A isThe sample injection rates of the component B are 239.1mL/min and 61.0mL/min respectively, the reaction time is 10min, the reaction product is stood for liquid separation, the water phase is recovered, and the oil phase is prepared by 5 wt% of Na2CO3And washing the aqueous solution to be neutral, and then carrying out liquid separation and rotary steaming to obtain the linseed oil polyol, wherein the hydroxyl value of the linseed oil polyol is 415mg KOH/g, and the viscosity of the linseed oil polyol is 8960 mPa.
Example 11:
dissolving 22.0L of epoxy castor oil in 66.0L of tetrahydrofuran to prepare component A, dissolving 1.8L of sulfuric acid in 36.0L of water to prepare component B, simultaneously pumping into a 6-stage series glass reaction kettle, wherein the reaction temperature of the kettle 1 is 45 ℃, the reaction temperature of the kettle 2 is 50 ℃, the reaction temperatures of the kettles 3, 4 and 5 are 55 ℃, the reaction temperature of the kettle 6 is 60 ℃, the sample injection rates of A, B components are 175.3mL/min and 74.6mL/min respectively, the reaction time is 12min, standing and separating the reaction products, recovering the water phase, and using 5 wt% of Na as an oil phase2CO3And (3) washing the aqueous solution to be neutral, and then carrying out liquid separation and rotary steaming to obtain the castor oil polyol, wherein the hydroxyl value of the castor oil polyol is 312mg KOH/g, and the viscosity of the castor oil polyol is 7150mPa & s.
Example 12:
dissolving 22.0L epoxy tung oil in 55.0L tetrahydrofuran to prepare component A, dissolving 1.7L sulfuric acid in 45.3L water to prepare component B, simultaneously pumping into a 6-stage series glass reaction kettle, wherein the reaction temperature of the kettle 1 is 40 ℃, the reaction temperatures of the kettles 2, 3 and 4 are 45 ℃, the reaction temperatures of the kettles 5 and 6 are 50 ℃, the sample injection rates of the A, B components are 132.8mL/min and 81.5mL/min respectively, the reaction time is 14min, standing the reaction products, recovering the water phase, using 5 wt% Na as the oil phase2CO3Washing the aqueous solution to be neutral, and then carrying out liquid separation and rotary evaporation to obtain the tung oil polyol, wherein the hydroxyl value of the tung oil polyol is 354mg KOH/g, and the viscosity of the tung oil polyol is 7680mPa & s.
Example 13:
dissolving 22.0L of epoxysafflower oil in 66.0L of tetrahydrofuran to prepare component A, dissolving 1.9L of sulfuric acid in 52.5L of water to prepare component B, simultaneously pumping into a 7-stage series glass reaction kettle, controlling the reaction temperature of kettles 1, 2, 3 and 4 at 30 ℃, the reaction temperature of kettles 5, 6 and 7 at 35 ℃, the sample injection rate of A, B components at 123.7mL/min and 70.7mL/min respectively, reacting for 18min, standing the reaction product for liquid separation, recovering the water phase, and using 5 wt% of Na as an oil phase2CO3Washing the water solution to be neutral, separating liquid, and performing rotary steaming to obtain safflower oil polyalcohol with a hydroxyl value of 303mg KOH/g and a viscosity of 6710mPa & s.
Example 14:
dissolving 22.0L of epoxy rice bran oil in 99.0L of tetrahydrofuran to prepare component A, dissolving 1.7L of sulfuric acid in 34.0L of water to prepare component B, simultaneously pumping into a 6-stage series glass reaction kettle, wherein the reaction temperature of the kettle 1 is 75 ℃, the reaction temperatures of the kettles 2 and 3 are 80 ℃, the reaction temperatures of the kettles 4 and 5 are 85 ℃, the reaction temperature of the kettle 6 is 90 ℃, the sample injection rates of A, B components are 233.4mL/min and 66.5mL/min respectively, the reaction time is 10min, standing and separating the reaction products, recovering the water phase, and using 5 wt% of Na as the oil phase2CO3Washing the aqueous solution to be neutral, separating liquid, and performing rotary steaming to obtain the rice bran oil polyol, wherein the hydroxyl value of the rice bran oil polyol is 275mg KOH/g, and the viscosity of the rice bran oil polyol is 6230mPa & s.
Example 15:
dissolving 22.0L epoxy corn oil in 44.0L tetrahydrofuran to prepare component A, dissolving 2.0L sulfuric acid in 50.0L water to prepare component B, simultaneously pumping into a 6-stage series glass reaction kettle, wherein the reaction temperature of the kettle 1 is 50 ℃, the reaction temperatures of the kettles 2, 3 and 4 are 55 ℃, the reaction temperatures of the kettles 5 and 6 are 60 ℃, the sample injection rates of A, B components are 165.4mL/min and 134.5mL/min respectively, the reaction time is 10min, separating the reaction products, standing, recovering the water phase, using 5 wt% Na as the oil phase2CO3Washing the aqueous solution to be neutral, and then carrying out liquid separation and rotary steaming to obtain the corn oil polyol, wherein the hydroxyl value of the corn oil polyol is 258mg KOH/g, and the viscosity of the corn oil polyol is 6410mPa & s.
Example 16:
dissolving 22.0L of epoxy tea oil in 55.0L of tetrahydrofuran to prepare component A, dissolving 1.5L of fluoboric acid in 27.9L of water to prepare component B, simultaneously pumping into an 8-stage series glass reaction kettle, wherein the reaction temperature of the kettle 1 is 30 ℃, the reaction temperatures of the kettles 2, 3, 4 and 5 are 35 ℃, the reaction temperatures of the kettles 6, 7 and 8 are 40 ℃, the sample injection rates of the A, B components are respectively 80.4mL/min and 33.5mL/min, the reaction time is 35min, standing and separating the reaction products, recovering the water phase, and using 5 wt% of Na as an oil phase2CO3Washing with water solution to neutrality, separating, and steaming to obtain tea oil polyalcohol with hydroxyl value of 227mg KOH/g and viscosityThe degree was 5490 mPas.
The epoxy value of the raw materials in the above examples is 6.0% -6.7%, and the epoxy value of the product epoxy vegetable oil is less than 0.1%, which shows that the conversion of epoxy groups is almost completely realized by using a multistage reaction kettle for amplification.
Comparative example 1:
as in example 8, the reaction vessel in the reaction apparatus was replaced with only one having no baffle plate and partition plate, and the results were: the pressure difference in the reaction kettle is more than 1 atmosphere, the glass reaction kettle material cannot bear the pressure difference, and the reaction cannot be carried out. Comparative example 2:
as in example 8, only the temperature was changed to 80 ℃ for the reaction in tank 1, 75 ℃ for the reaction in tanks 2, 3, 70 ℃ for the reaction in tanks 4, 5, 6 and 65 ℃ for the reaction in tank 7, with the results that: an epoxy value of 0.8%, a hydroxyl value of 152mg KOH/g and a viscosity of 14900 mPas.
Comparative example 3:
as in example 8, the baffle was changed to a right angle baffle having a side length of 1cm only, with the result that: the effusion in the reaction kettle is serious, the internal pressure difference is more than 1 atmosphere, the glass reaction kettle material cannot bear the pressure difference, and the reaction cannot be carried out.
Comparative example 4:
just the direction of the baffle was adjusted to be the same as in example 8, with the result that: after the baffle direction was transferred to unanimity, the mixed effect halved, and the inside pressure differential of reation kettle is greater than 1 atmospheric pressure, and the glass reation kettle material can't bear this pressure differential, and the reaction can't go on.
Comparative example 5:
CN103288642B 'a method for preparing vegetable oil polyalcohol by using a continuous method', is adopted to carry out small-scale amplification, 22.0L of epoxy olive oil is dissolved in 66.0L of tetrahydrofuran to prepare an A component, 1.4L of sulfuric acid is dissolved in 26.4L of water to prepare a B component, simultaneously, the mixture is pumped into a microchannel modular reaction device to react in a sandwich reactor HC at normal pressure and 50 ℃, the sample injection rates of A, B components are respectively 20.4mL/min and 6.56mL/min, the volume of a reactor in the microchannel modular reaction device is 2L, the reaction time is 75min, reaction products are stood for liquid separation,recovering water phase, and using 5% Na for oil phase2CO3Washing the aqueous solution to be neutral, and then carrying out liquid separation and rotary evaporation to obtain the olive oil polyalcohol with the epoxy value of 1.9%, the hydroxyl value of 166mgKOH/g and the viscosity of 9340mPa & s.
Claims (5)
1. The application of a reaction device in the continuous preparation of vegetable oil polyol is characterized in that the reaction device is formed by sequentially connecting a plurality of reaction kettles in series; wherein a jacket (2) is arranged outside the kettle body (1) of the reaction kettle; the reaction kettle is characterized in that a partition plate (3) is arranged in the kettle body (1) of the reaction kettle, a plurality of arc baffles (4) are arranged between every two adjacent partition plates (3), and the arc baffles (4) are fixed on the partition plates (3) at two sides;
wherein the directions of the upper and lower adjacent arc baffles are opposite;
wherein, the temperature of the post reaction kettle in the application is more than or equal to that of the front reaction kettle;
wherein the reaction device is formed by sequentially connecting 4-10 reaction kettles in series;
wherein, the reactor body (1) of the reaction kettle is internally provided with 5 layers of partition boards/0.5L, and the distance between every two layers of partition boards is 2 cm;
the central angle of the circular arc baffle (4) is 90 degrees, the radius is 1cm, and the thickness is 3 mm.
2. The application of claim 1, wherein the top of the kettle body (1) is respectively provided with a thermometer interface (5), a material inlet (8) and a pressure gauge interface (7); a material outlet (6) is formed in the bottom of the kettle body (1); the upper portion of the jacket lateral wall is provided with a hot coal outlet (9), the lower portion of the jacket lateral wall is provided with a heating medium inlet (10), and the bottom of the jacket is provided with an evacuation port (11).
3. The use according to claim 1, characterized in that the reaction apparatus further comprises a pump and a mixer, the two pumps are connected with the inlet of the mixer in parallel, the outlet of the mixer is connected to the material inlet (8) of the first reaction vessel, the material outlet (6) of the first reaction vessel is further connected with the material inlet (8) of the second reaction vessel, and the second reaction vessel to the tenth reaction vessel are connected in sequence according to the method.
4. The application of the method as claimed in claim 1, wherein the epoxy vegetable oil solution and the catalyst aqueous solution are respectively pumped into the mixer at the same time, are mixed and then are conveyed into the first reaction kettle from the material inlet (8) of the first reaction kettle to carry out a first reaction, and then are conveyed into the second reaction kettle from the material outlet (6) of the first reaction kettle through the material inlet (8) of the second reaction kettle to carry out a second reaction, and are sequentially reacted in the reaction kettles at different stages, and after the reaction in the last stage of reaction kettle is finished, the reaction liquid flows out from the material outlet (6) of the last stage of reaction kettle, and the effluent liquid is collected.
5. The application of the epoxy vegetable oil solution as claimed in claim 4, wherein the solvent of the epoxy vegetable oil solution is any one or combination of tetrahydrofuran, pyridine, acetone and methyl isobutyl ketone, and the volume ratio of the epoxy vegetable oil to the solvent is 1: 1.5-8; the volume ratio of the catalyst to water in the catalyst aqueous solution is 1: 15-40; controlling the use amount of the epoxy vegetable oil solution and the catalyst water solution to ensure that the volume ratio of the epoxy vegetable oil to the catalyst is 1: 10-20; the reaction time is 10-40 min, and the reaction temperature is 30-100 ℃.
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