CN115845775A - Polymer synthesis reaction device capable of continuously atomizing and sampling - Google Patents
Polymer synthesis reaction device capable of continuously atomizing and sampling Download PDFInfo
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Abstract
The invention discloses a polymer synthesis reaction device for continuous atomization and sample introduction, and relates to the field of chemical reaction synthesis devices. The device consists of a reaction part with heating, stirring and atmosphere protection and a continuous atomization sample introduction part, wherein an atomization solvent required by the reaction is continuously blown into the reaction device through gas with certain pressure. The device can ensure the safety of adding the solvent or reactant in the high-temperature synthesis process under the inert atmosphere condition, can reduce the temperature change of a reaction system during sample injection by a mode of driving continuous atomization sample injection through gas-phase purging, can fully mix the reactant and the solvent, can control the sample injection rate of the solvent or the reactant by adjusting the air input and the atomization amount, and further controls the reaction rate.
Description
Technical Field
The invention relates to the field of polymer synthesis in the field of chemistry and chemical engineering, in particular to a polymer synthesis reaction device for continuous atomization and sample injection.
Background
Chemical reaction synthesis is the basis of all chemical applications, conditions such as high temperature, high pressure, inert atmosphere protection and the like are usually involved in chemical reaction, and reasonable design of a chemical reaction device is very critical to reaction synthesis. Taking the organic polymer synthesis reaction as an example, the reaction often involves heating at a higher temperature, stirring, protection by an inert atmosphere, and addition of reactants during the reaction (chem.eng.j., 2021,418, 129311.) to synthesize the polymer: molecular weight, molecular weight distribution, molecular polymerization form, etc. are closely related to experimental details such as viscosity and temperature of the reaction system (macromol., 2020,53, 569-583), and the difficulty and danger of operation during the reaction process are also a test for the experimental operator, and how to design a reactor satisfying the above requirements and considering the simplicity and safety of experimental operation is very important for chemical reaction synthesis. Therefore, the invention aims to invent a polymer synthesis reaction device with continuous atomization and sample introduction.
Disclosure of Invention
The invention provides a polymer synthesis reaction device for continuous atomization sample introduction, which can ensure the safety of adding a solvent or a reactant in a high-temperature synthesis process under the condition of inert atmosphere, can reduce the temperature change of a reaction system during sample introduction by a mode of driving continuous atomization sample introduction through gas-phase purging, can fully mix the reactant and the solvent, can control the sample introduction rate of the solvent or the reactant by adjusting the air input and the atomization amount, and further controls the reaction rate.
The specific technical scheme of the invention is as follows: in order to achieve the purpose, the technical scheme of the invention is a polymer synthesis reaction device with continuous atomization and sample introduction, which comprises a magnetic stirrer (1), an oil bath pot (2), a three-mouth flask (3), a magneton (4), an aeration pipe (5), a reactant and a solvent (6), a return pipe (7), a water separator (8), a gas phase inlet (9), a gas phase outlet (10), a gas cylinder (11), a pressure reducing valve (12), an atomizer (13), a gas phase pipeline (14), a protective gas cylinder (15), a gas flowmeter (16) and a wash bottle (17).
The gas cylinder (11) is connected with a pressure reducing valve (12), the pressure reducing valve (12) is connected with an atomizer (13) through a gas phase pipeline (14), the atomizer (13) is connected with an aerator pipe (5) through the gas phase pipeline (14), the aerator pipe (5) is connected with the three-neck flask (3), and the aerator pipe (5) is inserted below the liquid level of a reactant and a solvent (6) so as to ensure that a gas phase in a system is discharged from a gas phase outlet (10) to a wash bottle (17) when the reaction device operates. Magnetic stirrers (1) and oil bath pot (2) make up the oil bath that has the magnetic stirring function, three-neck flask (3) are fixed in oil bath pot (2) and magnetic stirrers (1) top, magneton (4) and reactant + solvent (6) have been put to the inside of three-neck flask (3), three-neck flask (3) are connected with water knockout drum (8), water knockout drum (8) are connected with back flow (7), the back flow is connected with gaseous phase export (10), gaseous phase export (10) are connected with wash flask (17). The protective gas bottle (15) is connected with a gas flowmeter (16), and the gas flowmeter (16) is connected with the three-neck flask (3) through a gas phase pipeline (14).
The protective gas bottle (15) and the gas flowmeter (16) can provide a constant flow inert atmosphere condition: inert gas is controlled by a gas flowmeter (16), and is introduced into the three-neck flask (3) through a gas phase pipeline (14), an aeration pipe (5) below the liquid level of the reactant and the solvent (6) is inserted to avoid feeding failure caused by protective gas entering a feeding gas circuit, the protective gas blows and sweeps the reaction device after entering the three-neck flask (3), and air in the device is discharged from a gas phase outlet (10) to a washing bottle (17) through a water separator (8) and a return pipe (7) which are connected with the three-neck flask (3) in sequence and is discharged after being washed.
The gas bottle (11) is opened, the pressure reducing valve (12) is adjusted, the gas in the gas bottle enters the three-mouth flask (3) through the gas phase pipeline (14) and the atomizer (13), and the air in the pipeline is discharged. When the polymerization reaction begins to occur, the atomizer (13) is opened, and the solvent required for the reaction is added into the atomizer (13). The solvent is atomized and then blown into the three-neck flask (3) through the gas phase in the gas phase pipeline (14) to participate in the polymerization reaction. The method can realize polymer synthesis in a closed system under the conditions of inert atmosphere and high-temperature synthesis, and avoid environmental pollution caused by the escape of high-temperature organic steam during midway feeding, safety risks of manual operation under the high-temperature condition and adverse influence of outside air entering a reaction system on a synthetic product. The water separator (8) connected with the three-mouth flask (3) can collect small molecular products generated in the polymerization reaction, so that the whole polymerization reaction is carried out in the positive direction, the synthesis efficiency of the polymer is improved, the reflux pipe (7) can condense and reflux the solvent steam evaporated at high temperature, the utilization rate of the solvent is improved, and resources are saved.
When the polymerization reaction is fed, the gas flow of the pressure reducing valve (12) and the atomization amount of the atomizer (13) can be controlled to continuously feed, the atomized solvent can continuously and stably enter the three-neck flask (3) through the gas phase pipeline (14), so that the solvent is fully contacted with the reaction system, and for a polymer reaction system sensitive to the reaction temperature of the system, compared with the traditional uncapping feeding, the continuous atomized solvent entering system can greatly reduce the influence on the reaction system due to the temperature change, and the reaction efficiency and the product quality are improved.
The invention has the advantages that: 1. the atomized solvent is blown into a high-temperature reaction system through gas phase, so that the environmental pollution caused by the escape of organic steam when the cover is opened for feeding is avoided, and the safety of manual operation is ensured; 2. the reaction solvent enters the reaction system in the form of atomized solvent, so that the temperature change of the reaction system during feeding can be reduced; 3. the atomized solvent can be fully mixed with reactants and solvent in the reaction system; 4. the feeding speed of the solvent can be controlled and the continuous and stable feeding effect can be realized by adjusting the air inflow in the feeding air circuit and the atomization amount of the atomizer; 5. the reaction device has simple design structure and convenient installation, and can effectively save resources.
The gas phase is provided by a protective gas bottle (15) and a gas bottle (11), the gas in the protective gas bottle (15) is regulated by a gas flowmeter (16) and then provides protective gas for the whole reaction device, so that the polymer synthesis reaction is carried out under the inert atmosphere condition, and the gas is discharged to a washing bottle (17) through a gas phase outlet (10) and then discharged after being washed.
The aeration pipe (5) is inserted below the liquid level of the reactant and the solvent (6) in the three-neck flask (3) to prevent protective gas in a reaction device from entering the atomizer (13) from the aeration pipe (5), and the liquid phase in the three-neck flask (3) has a certain height so that the magneton (4) at the bottom of the three-neck flask (3) does not collide with the aeration pipe (5) during rotation.
The gas bottle (11) and the pressure reducing valve (12) are combined to form a gas source capable of adjusting output pressure, gas provided by the gas source can push the atomized solvent in the atomizer (13) to enter the three-neck flask (3) through the gas phase pipeline (14) and the aeration pipe (5), and meanwhile, the gas pressure is slightly greater than the protective gas pressure in the three-neck flask (3) so as to ensure that the atomized solvent generated in the atomizer (13) can enter the three-neck flask (3).
The internal pressure of the reaction device is slightly greater than the atmospheric pressure, and the specific pressure is 1.1-2.0 atmospheric pressure, so as to ensure that the internal pressure of the reaction device is positive pressure, and the specific expression is that when gas is discharged from the gas phase outlet (10) into the gas washing bottle (17), bubbles appear in the bottle.
The working temperature of the reaction device is between room temperature and 200 ℃.
The reactant of the reaction device is powder or solution or suspension dispersed in liquid phase solvent. The reaction system contains at least a liquid phase.
The liquid phase solvent comprises inorganic solvent water, water salt solution and organic matter/water solution which is mutually soluble with water in any proportion, the organic solvent is C6-C20 hydrocarbon, aromatic hydrocarbon, substituted hydrocarbon, alcohol, ketone, ether, ester, phosphine and amine liquid phase organic compound, wherein the organic solvent also comprises one or more of surfactants which are mixed with C6-C20 and contain carboxyl and sulfonic acid groups, primary amine, secondary amine, tertiary amine and quaternary ammonium salt, and hydrocarbon oxime, and the compound is used as a reactant
Such gases, including inert working gases such as nitrogen, argon; also included are precipitating reactive gases such as carbon dioxide; and redox gases such as ozone, hydrogen, and oxygen.
Drawings
FIG. 1 is a schematic diagram of a polymer synthesis reaction device with continuous atomization and sample injection: in the figure: 1. the device comprises a magnetic stirrer, 2, an oil bath, 3, a three-neck flask, 4, a magneton, 5, an aeration pipe, 6, a reactant and a solvent, 7, a return pipe, 8, a water separator, 9, a gas phase inlet, 10, a gas phase outlet, 11, a gas cylinder, 12, a pressure reducing valve, 13, an atomizer, 14, a gas phase pipeline, 15, a protective gas cylinder, 16, a gas flowmeter, 17 and a washing bottle.
FIG. 2 is a gel permeation chromatogram of the intrinsically microporous polymer PIM-1 of example 1 according to the invention.
FIG. 3 is a gel permeation chromatogram of the intrinsically microporous polymer PIM-1 of example 2 of the present invention.
FIG. 4 is a gel permeation chromatogram of the intrinsically microporous polymer PIM-1 of example 3 of the present invention.
Detailed Description
The operation flow of the polymer synthesis reaction device with continuous atomization and sample injection is described by combining the attached figure 1 as follows:
s1, adding a reactant and a solvent (6) into a three-neck flask (3), inserting an aeration pipe (5) below the liquid level of the reactant and the solvent (6), and introducing cooling water into a return pipe (7).
S2, opening the protective gas bottle (15), adjusting the gas flow of the gas flowmeter (16), introducing the protective gas, purging in the device, and discharging the air in the system.
S3, opening the gas cylinder (11), adjusting the pressure reducing valve (12) to enable the gas in the gas cylinder to purge the air in the gas phase pipeline (14), and discharging the air through the gas phase outlet (10) and the washing bottle (17).
S4, turning on the magnetic stirrer (1) to adjust the stirring rate, turning on the oil bath (2) to adjust the temperature, and starting the reaction of the reactants in the flask after the temperature rises.
And S5, after the reaction is carried out for a period of time, the viscosity of the reactant and the solvent (6) in the flask (3) rises, the atomizer (13) is started, the atomization amount is adjusted, and the atomized solvent discharged from the atomizer (13) is blown into the flask (3) from a gas phase pipeline (14) by a gas phase in the gas cylinder (11).
And S6, after the reaction is finished, closing the atomizer (13), the gas cylinder (11), the pressure reducing valve (12), the protective gas cylinder (15), the gas flowmeter (16), the oil bath and the magnetic stirrer (1), disassembling the reaction device, and taking out a product after the reaction for subsequent treatment.
The present invention is further described in detail below by way of specific examples, which enable a person skilled in the art to more fully understand the invention, without in any way limiting it.
The intrinsic microporous polymer PIM-1 adopted in the examples is synthesized by a high-temperature method under the protection of nitrogen atmosphere, the synthesized PIM-1 has the weight-average molecular weight Mw of 150-200kDa and the polydispersity coefficient PDI of 1.7-2.2.
Example 1:
in this example, the intrinsic microporous polymer PIM-1 was synthesized using the above synthesis reaction apparatus, and the specific synthesis steps were as follows:
1.0g (5 mmol) of polymer monomer tetrafluoroterephthalonitrile (TFTPN), 1.7g (5 mmol) of 5,5', 6' -tetrahydroxy-3, 3 '-tetramethyl-1, 1' -helical bisindane (TTSBI) and potassium carbonate (K) serving as a catalyst 2 CO 3 ) 2.07g (15 mmol) were placed in a three-necked flask and kept under a continuous nitrogen gas flow for about 20min.
10ml of N, N-dimethylacetamide (DMAc) and 5ml of toluene were sucked up by a medical syringe and slowly injected into a three-necked flask with an aeration tube located below the mixture solvent level, and aeration was started.
The magnetic stirrer was turned on, the stirring rate was adjusted to 200rpm, the oil bath temperature was set to 150 ℃, heating was started, and the reaction time was maintained for about 60min.
Along with the continuous polymerization process of the polymer monomer, the solution viscosity continuously rises, at the moment, a reflux solvent appears in the water separator, the stirring speed is increased to 500rpm (at the moment, the reaction time is about 5min, and the torque is about 2N/cm), the atomizer is opened, the atomization amount is adjusted to be 0.4ml/min, and the toluene solvent in the atomizer is blown into the three-neck flask through nitrogen.
And after the reaction, the reaction device is detached while the reaction device is hot, and the yellow viscous liquid in the three-neck flask is poured into methanol to obtain a yellow solid. And dissolving the solid after suction filtration in Tetrahydrofuran (THF), dropwise adding methanol for recrystallization, and washing the solid with methanol and distilled water sequentially for three times to obtain the product PIM-1. The yield thereof was found to be 48%.
As shown in FIG. 2, the synthesized PIM-1 had a molecular weight Mw of 158.5kDa and a polydispersity index PDI of 2.0 as determined by gel permeation chromatography.
Example 2:
this example is similar to the procedure of example 1, except that:
the atomization amount is controlled to be 0.6ml/min, and the total reaction time is 40min. Collecting and post-treating the purified product PIM-1. The yield thereof was found to be 30%.
As shown in FIG. 3, the synthesized PIM-1 had a molecular weight Mw of 195.8kDa and a polydispersity index PDI of 1.7 as determined by gel permeation chromatography.
Example 3:
this example is similar to the procedure of example 1, except that:
the atomization amount is controlled to be 0.3ml/min, and the total reaction time is 80min. Collecting and post-treating purified product PIM-1. The yield thereof was found to be 38%.
As shown in FIG. 4, the synthesized PIM-1 had a molecular weight Mw of 157.1kDa and a polydispersity index PDI of 2.2 as determined by gel permeation chromatography.
In examples 1-3, continuous, stable, controlled preparation of the intrinsically microporous polymer PIM-1 of different molecular weights and molecular weight distributions was achieved by adjusting the condition parameters of the present invention. The toluene enters the reaction system in an atomized form, so that the temperature change of the reaction system during feeding can be reduced, the toluene is uniformly mixed with the reaction system, the problem of difference of different batches in the synthesis process of the microporous polymer can be further reduced, and a feasible scheme is provided for the synthesis process and large-scale production of the microporous polymer.
The above-mentioned embodiment is only a preferred solution of the present invention, and is not intended to limit the present invention. It should be noted that, for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can be made, and such improvements and modifications should also be considered as the protection scope of the present invention.
Claims (8)
1. A polymer synthesis reaction device for continuous atomization and sample introduction is characterized in that: the device comprises a magnetic stirrer (1), an oil bath pot (2), a three-neck flask (3), a magneton (4), an aeration pipe (5), a reactant and solvent (6), a backflow pipe (7), a water separator (8), a gas phase inlet (9), a gas phase outlet (10), a gas cylinder (11), a pressure reducing valve (12), an atomizer (13), a gas phase pipeline (14), a protective gas cylinder (15), a gas flowmeter (16) and a washing bottle (17);
the gas cylinder (11) is connected with a pressure reducing valve (12), the pressure reducing valve (12) is connected with an atomizer (13) through a gas phase pipeline (14), the atomizer (13) is connected with an aerator pipe (5) through the gas phase pipeline (14), the aerator pipe (5) is connected with the three-neck flask (3), and the aerator pipe (5) is inserted below the liquid level of a reactant and a solvent (6) so as to ensure that a gas phase in a system is discharged from a gas phase outlet (10) to a wash bottle (17) when the reaction device operates; the magnetic stirrer (1) and the oil bath pot (2) are combined into an oil bath with a magnetic stirring function, the three-mouth flask (3) is fixed above the oil bath pot (2) and the magnetic stirrer (1), a magneton (4) and a reactant and a solvent (6) are placed inside the three-mouth flask (3), the three-mouth flask (3) is connected with a water distributor (8), the water distributor (8) is connected with a return pipe (7), the return pipe is connected with a gas phase outlet (10), and the gas phase outlet (10) is connected with a washing bottle (17); the protective gas bottle (15) is connected with a gas flowmeter (16), and the gas flowmeter (16) is connected with the three-neck flask (3) through a gas phase pipeline (14);
the protective gas bottle (15) and the gas flowmeter (16) provide a constant flow inert atmosphere condition: inert gas is controlled by a gas flowmeter (16), an aeration pipe (5) below the liquid level of a reactant and a solvent (6) is inserted into the three-neck flask (3) through a gas phase pipeline (14) to avoid feeding failure caused by protective gas entering a feeding gas circuit, the protective gas blows and sweeps the reaction device after entering the three-neck flask (3), and air in the device is discharged from a gas phase outlet (10) to a washing bottle (17) through a water separator (8) and a return pipe (7) which are connected with the three-neck flask (3) in sequence and is discharged after being washed.
2. The method for applying the polymer synthesis reaction device with the continuously atomized sample introduction according to claim 1, wherein the method comprises the following steps: opening a gas bottle (11), adjusting a pressure reducing valve (12), allowing gas in the gas bottle to enter a three-neck flask (3) through a gas phase pipeline (14) and an atomizer (13), and discharging air in the pipeline; when the polymerization reaction starts to occur, opening an atomizer (13), and adding a solvent required by the reaction into the atomizer (13); after being atomized, the solvent is blown into the three-neck flask (3) through the gas phase in the gas phase pipeline (14) to participate in the polymerization reaction;
a water separator (8) connected with the three-neck flask (3) collects micromolecule products generated in the polymerization reaction, and a return pipe (7) condenses and returns solvent vapor evaporated at high temperature;
when the polymerization reaction is fed, the gas flow of the pressure reducing valve (12) and the atomization amount of the atomizer (13) are controlled to continuously feed, and the atomized solvent continuously and stably enters the three-neck flask (3) through the gas phase pipeline (14) to fully contact with the reaction system;
the gas phase is provided by a protective gas bottle (15) and a gas bottle (11), the gas in the protective gas bottle (15) is regulated by a gas flowmeter (16) to provide protective gas for the whole reaction device, so that the polymer synthesis reaction is carried out under the condition of inert atmosphere, and the gas is discharged to a washing bottle (17) through a gas phase outlet (10) and is discharged after being washed;
the aeration pipe (5) is inserted below the liquid level of the reactant and the solvent (6) in the three-neck flask (3) to prevent protective gas in a reaction device from entering the atomizer (13) from the aeration pipe (5), and the liquid phase in the three-neck flask (3) has a certain height so that the magneton (4) at the bottom of the three-neck flask (3) does not collide with the aeration pipe (5) during rotation.
3. The method of claim 2, wherein: the gas bottle (11) and the pressure reducing valve (12) are combined to form a gas source capable of adjusting output pressure, gas provided by the gas source pushes the atomized solvent in the atomizer (13) to enter the three-mouth flask (3) through the gas phase pipeline (14) and the aerator pipe (5), and meanwhile, the gas pressure is slightly greater than the protective gas pressure in the three-mouth flask (3) so as to ensure that the atomized solvent generated in the atomizer (13) enters the three-mouth flask (3).
4. The method of claim 2, wherein: the internal pressure of the reaction device is 1.1-2.0 atmospheric pressure, so as to ensure that the interior of the reaction device is in positive pressure, and the specific expression is that when gas is discharged from a gas phase outlet (10) into a gas washing bottle (17), bubbles appear in the bottle.
5. The method of claim 2, wherein: the working temperature is between room temperature and 200 ℃.
6. The method of claim 2, wherein: the reactant is powder or solution or suspension dispersed in liquid phase solvent; the reaction system at least contains a liquid phase;
the liquid phase solvent comprises inorganic solvent water, water salt solution and organic matter/water solution which is mutually soluble with water in any proportion, the organic solvent is C6-C20 hydrocarbon, aromatic hydrocarbon, substituted hydrocarbon, alcohol, ketone, ether, ester, phosphine and amine liquid phase organic compound, wherein the organic solvent also comprises one or more of surfactant and hydrocarbon oxime which are mixed with C6-C20 and contain carboxyl and sulfonic group, and primary amine, secondary amine, tertiary amine and quaternary ammonium salt.
7. The method of claim 2, wherein: the gas comprises inert working gas and precipitating reaction gas; redox gases are also included.
8. The method for applying the polymer synthesis reaction device with the continuous atomized sample injection as claimed in claim 1, which is characterized by comprising the following operation procedures:
s1, adding a reactant and a solvent (6) into a three-neck flask (3), inserting an aeration pipe (5) below the liquid level of the reactant and the solvent (6), and introducing cooling water into a return pipe (7);
s2, opening a protective gas bottle (15), adjusting a gas flow meter (16) to a proper gas flow, introducing protective gas, purging in the device, and discharging air in the system;
s3, opening the gas cylinder (11), adjusting the pressure reducing valve (12) to enable gas in the gas cylinder to purge air in the gas phase pipeline (14), and discharging the air through the gas phase outlet (10) and the washing bottle (17);
s4, turning on the magnetic stirrer (1) to adjust stirring speed, turning on the oil bath (2) to adjust temperature, and starting reaction of reactants in the flask after the temperature rises;
s5, after reacting for a period of time, the viscosity of the reactant and the solvent (6) in the flask (3) rises, the atomizer (13) is started, the atomization amount is adjusted, and the atomized solvent discharged by the atomizer (13) is blown into the flask (3) from a gas phase pipeline (14) by a gas phase in the gas cylinder (11);
and S6, after the reaction is finished, closing the atomizer (13), the gas cylinder (11), the pressure reducing valve (12), the protective gas cylinder (15), the gas flow meter (16), the oil bath and the magnetic stirrer (1), disassembling the reaction device, and taking out a product after the reaction for subsequent treatment.
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