CN111545148B - Chiral catalysis method and catalytic device thereof - Google Patents
Chiral catalysis method and catalytic device thereof Download PDFInfo
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- CN111545148B CN111545148B CN202010266174.8A CN202010266174A CN111545148B CN 111545148 B CN111545148 B CN 111545148B CN 202010266174 A CN202010266174 A CN 202010266174A CN 111545148 B CN111545148 B CN 111545148B
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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
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B53/00—Asymmetric syntheses
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D209/02—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom condensed with one carbocyclic ring
- C07D209/04—Indoles; Hydrogenated indoles
- C07D209/10—Indoles; Hydrogenated indoles with substituted hydrocarbon radicals attached to carbon atoms of the hetero ring
- C07D209/18—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D209/20—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals substituted additionally by nitrogen atoms, e.g. tryptophane
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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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J2219/12—Processes employing electromagnetic waves
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
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Abstract
The invention discloses a chiral catalysis method and a catalysis device thereof. The chiral catalysis method comprises the steps of generating millimeter-scale electromagnetic waves, forming a standing wave resonance area at a raw material position through the electromagnetic waves, then adjusting the propagation direction of electromagnetic standing waves in the standing wave resonance area and the electric field intensity, and generating a chiral compound after reaction. The chiral catalytic device of the present invention comprises: the reaction cavity is used for placing raw materials; an electrode assembly, the end of which extends into the reaction chamber; the pulse power supply is electrically connected with the electrode assembly to promote the electrode assembly to generate millimeter-scale electromagnetic waves in the reaction cavity; and the coil is spirally wound outside the reaction cavity body. The invention solves the problem of overhigh cost of synthesizing chiral molecules by the existing chemical chiral catalyst, and the plasma catalysis of the invention replaces the common chemical chiral catalyst, so that a high-purity product can be obtained on the premise of no need of separation and purification, and the cost is effectively reduced.
Description
Technical Field
The invention relates to the field of chemical engineering, and relates to a catalytic method and a catalytic device for a chiral material.
Background
The chiral compound is synthesized by a traditional method, a mixture of two chiral molecules is always obtained, and a complex chiral resolution method is needed, namely, a left-handed molecule and a right-handed molecule are separated to obtain a single chiral molecule. This is costly and wasteful. At present, in order to save cost, the best mode adopted is to use a chemical chiral catalyst to automatically identify chirality, so that the reaction only takes place to one path, and only molecules with specific chirality are generated.
However, the existing chemical chiral catalysts have the problems of low efficiency, difficult degradation and the like. Therefore, in the process of synthesizing product molecules, more catalyst molecules are often required for synthesis, and thus the synthesis cost is high. In addition, the catalytic molecules and the product molecules need to be separated at the later stage, so that the synthesis procedures are increased, and the production cost is further increased.
Disclosure of Invention
The invention aims to solve the problem that the cost for synthesizing chiral molecules by using the existing chemical chiral catalyst is too high; the invention provides a chiral catalysis method and a chiral catalysis device which can effectively reduce the synthesis cost.
A chiral catalytic process comprising:
generating millimeter-scale electromagnetic waves, forming a standing wave resonance area at the position of the raw material through the electromagnetic waves, then adjusting the propagation direction and the electric field intensity of electromagnetic standing waves in the standing wave resonance area, and generating a chiral compound after reaction.
The electromagnetic wave in the standing wave resonance region is millimeter-scale electromagnetic wave.
The process of adjusting the propagation direction and the electric field strength of the electromagnetic standing wave in the standing wave resonance region is as follows: adjusting the current direction to form an electromagnetic standing wave propagation direction corresponding to the chiral direction, and adjusting the electric field strength of the standing wave resonance region to be more than 10^ 3V/m.
The raw materials are synthesized under the condition of working gas, and the working gas is argon.
A chiral catalytic device, comprising:
the reaction cavity is used for placing raw materials;
an electrode assembly, one end of which extends into the reaction chamber;
the pulse power supply is electrically connected with the electrode assembly and is used for promoting the electrode assembly to generate millimeter-scale electromagnetic waves in the reaction cavity and forming a standing wave resonance area in the reaction cavity;
the coil is spirally wound outside the reaction cavity, the propagation direction of the electromagnetic standing wave in the standing wave resonance region is adjusted by adjusting the current direction of the control coil, and the control of the chiral direction can be realized by adjusting the propagation direction of the electromagnetic standing wave to the direction corresponding to the chiral direction.
The electrode assembly includes an electrode and a dielectric disposed on a surface of the electrode.
The electrode is made of copper; the dielectric body is made of ceramic; the reaction cavity is made of quartz.
The reaction cavity is of a tubular structure, one end of the electrode assembly is fixed at one end of the reaction cavity, and the other end of the electrode assembly is of a conical structure; the central axis of the electrode assembly is superposed with the central axis of the reaction cavity; the coil is fixed on the outer wall of the tubular structure.
The diameter of the outer wall of the reaction cavity is 6-10mm, and the length of an electrode assembly positioned in the reaction cavity is 10-20 mm; the coil is a single-spiral coil, and the pitch L between two adjacent spirals in the single-spiral coil is 40-60 mm.
The wavelength range of the electromagnetic waves is 1-10 mm; the electric field intensity of the coil is more than 10^ 3V/m.
The reaction cavity is also communicated with a gas inlet, and the protective gas can be introduced through the gas inlet, so that the reaction cavity is suitable for the generation of a product which needs the protective gas in the reaction of raw materials; the reaction cavity is also communicated with a raw material pump, so that the raw material can be effectively input or output through the raw material pump, and the operation is simpler and more convenient.
The technical scheme of the invention has the following advantages:
1. the invention provides a chiral catalysis method, which shows that: the method can use the control of millimeter-scale electromagnetic waves to replace chemical catalytic reagents, a standing wave resonance area is formed at the position of the raw material through the millimeter-scale electromagnetic waves, then the propagation direction of electromagnetic standing waves and the electric field intensity in the standing wave resonance area are adjusted, and the chiral compound can be generated after the reaction. The method simplifies the preparation process of the single chiral compound, the prepared product has extremely high purity, the separation operation between the catalyst and the product is not needed, the process steps are greatly simplified, and meanwhile, the single chiral compound prepared by the method has extremely high efficiency and very obvious effect.
2. The method can effectively generate the target product in the standing wave resonance region theoretically if the wavelength range of the electromagnetic wave is millimeter-sized, the strength of an electric field in the standing wave resonance region is not particularly required, the wavelength range of the electromagnetic wave and the strength of the electric field in the standing wave resonance region are further optimized on the basis of the theory, namely, the wavelength range of the electromagnetic wave is preferably 1-10 mm, the electric field strength of the coil is preferably more than 10^3V/m, the target product can be effectively generated in about 1h through the limitation of the condition, the purity of the target product can reach more than 98%, and the effect is more remarkable.
3. The invention discloses a chiral catalytic device which mainly comprises a reaction cavity, an electrode assembly, a pulse power supply and a coil. When the device is used, raw materials are only required to be placed in the reaction cavity, the raw materials are excited by the pulse power supply to act on the electrode assembly, the electrode assembly generates millimeter-scale electromagnetic waves, the millimeter-scale electromagnetic waves form a standing wave resonance area in the reaction cavity, then the propagation direction of electromagnetic standing waves in the standing wave resonance area is adjusted and controlled through an electric field generated by an additional coil, and finally the generation of a target chiral compound is guided in the reaction cavity through electromagnetic standing waves in a specific direction. After the device is used, a chemical catalytic agent is not required to be added, and a single chiral compound can be effectively generated through the regulation and control of electromagnetic waves and an electric field, so that the production cost is greatly reduced. In addition, the raw materials in the invention can be generated in a larger reaction cavity, so that the synthesis efficiency of the compound with single chirality is greatly improved, and the effect is very obvious.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic view of the structure of the present invention;
description of the reference numerals:
1-a reaction cavity, 2-an electrode assembly, 3-a pulse power supply, 4-a coil, 5-a gas inlet and 6-a raw material pump.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
Example 1
A chiral catalytic device comprises a reaction cavity 1, an electrode assembly 2, a pulse power supply 3 and a coil 4. The reaction chamber 1 is a quartz tube, and the electrode assembly 2 is composed of an electrode made of a copper material and a dielectric made of a ceramic material, and the dielectric is disposed on an outer layer of the electrode, as shown in fig. 1. One end of the electrode assembly 2 is fixed on the reaction cavity 1 and is electrically connected with the pulse power supply 3, the other end of the electrode assembly 2 extends into the reaction cavity 1, and the central axis of the reaction cavity 1 is coincided with the central axis of the electrode assembly 2. The coil 4 is wound and fixed on the outer wall of the reaction cavity 1. The diameter of the outer wall of the reaction cavity 1 is 8mm, the length of the electrode assembly 2 positioned in the reaction cavity 1 is 15mm, and the diameter of the electrode assembly is 2mm, namely the diameter of the inner wall of the reaction cavity 1 is larger than 2 mm; the coil 4 is a single spiral coil, and the pitch L between two adjacent spirals in the coil is 50mm, as shown in fig. 1. Meanwhile, the reaction chamber 1 is also provided with a gas inlet 5 which is communicated with a pump 6.
The method for carrying out catalytic synthesis by adopting the catalytic device comprises the following steps: in the present example, a B-L-tryptophan ester monomer was used as a raw material to synthesize polyhydroxyethylindolpropanate (PIPEMA).
Step one, putting 0.5g of raw material B-L-tryptophan ester monomer into a reaction cavity 1, and introducing working gas from a gas inlet 5, wherein the working gas is argon, and the gas introduction amount is 0.1L;
and step two, starting the pulse power supply 3, adjusting the voltage of the pulse power supply 3 to enable the electrode assembly 2 to generate 1mm electromagnetic waves in the reaction cavity 1, wherein the electromagnetic waves are generated in the quartz tube, so that the electromagnetic waves form a standing wave resonance region in the quartz tube.
And step three, adjusting the electric field of the coil, specifically adjusting the electric field to a polar electric field of 10^4V/m, and obtaining 0.1g of finished product after 60min, wherein part of the unharvested raw materials are mixed in the working gas.
And detecting that the final product obtained in the third step has a main chain with dominant chiral helical conformation accounting for 99 percent of the total weight of the final product.
Example 2
A chiral catalytic method adopts the catalytic device in example 1 to perform catalytic synthesis, and in this example, adopts B-L-tryptophan ester monomer raw materials to synthesize polyhydroxyethylindole methacrylate (PIPEMA).
The method specifically comprises the following steps:
step one, putting 0.5g of raw material B-L-tryptophan ester monomer into a reaction cavity 1, and introducing working gas from a gas inlet 5, wherein the working gas is helium, and the gas introduction amount is 0.1L;
and step two, starting the pulse power supply 3, adjusting the voltage of the pulse power supply 3 to enable the electrode assembly 2 to generate 10mm electromagnetic waves in the reaction cavity 1, wherein the electromagnetic waves are generated in the quartz tube, so that the electromagnetic waves form a standing wave resonance region in the quartz tube.
Step three, adjusting the electric field of the coil 4, specifically to a polar direction electric field of 10^5V/m, and obtaining a finished product with the weight of 0.2g after 60 min; wherein part of the non-harvested material is entrained in the working gas.
As a result of the examination, it was found that, in the final product obtained in step three, the product having the helical conformation in which the main chain exhibited the dominant chirality accounted for 98% of the total amount of the final product.
The raw materials mixed in the working gas in the above examples 1 and 2 can be recycled, thereby reducing the waste of the raw materials.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (8)
1. A chiral catalytic process, comprising:
generating millimeter-level electromagnetic waves, forming a standing wave resonance area at the position of the raw material through the electromagnetic waves, then adjusting the propagation direction and the electric field intensity of electromagnetic standing waves in the standing wave resonance area, and generating a chiral polymer after reaction;
the wavelength range of the electromagnetic waves is 1-10 mm;
the process of adjusting the propagation direction and the electric field strength of the electromagnetic standing wave in the standing wave resonance region is as follows: adjusting the current direction to form an electromagnetic standing wave propagation direction corresponding to the chiral direction, and adjusting the electric field strength of the standing wave resonance region to be more than 10^ 3V/m.
2. The method of claim 1, wherein the feedstock is synthesized with a working gas that is argon.
3. A chiral catalytic device based on a chiral catalytic process according to claim 1 or 2, comprising:
the reaction cavity (1) is used for placing raw materials;
an electrode assembly (2), one end of which extends into the reaction chamber (1);
the pulse power supply (3) is electrically connected with the electrode assembly (2) and is used for promoting the electrode assembly (2) to generate millimeter-grade electromagnetic waves in the reaction cavity (1);
and the coil (4) is spirally wound outside the reaction cavity (1).
4. Chiral catalytic device according to claim 3, characterized in that the electrode assembly (2) comprises an electrode and a dielectric arranged at the surface of the electrode.
5. The chiral catalytic device of claim 4, wherein the electrode is made of copper; the dielectric body is made of ceramic; the reaction cavity (1) is made of quartz.
6. The chiral catalytic device according to any one of claims 3 to 5, wherein the reaction chamber (1) has a tubular structure, one end of the electrode assembly (2) is fixed at one end of the reaction chamber (1), and the other end of the electrode assembly (2) has a conical structure; the central axis of the electrode assembly (2) is superposed with the central axis of the reaction cavity (1); the coil (4) is fixed on the outer wall of the tubular structure.
7. The chiral catalytic device according to claim 6, wherein the outer wall of the reaction chamber (1) has a diameter of 6-10mm, and the electrode assembly (2) located in the reaction chamber (1) has a length of 10-20 mm; the coil (4) is a single-spiral coil, and the pitch L between two adjacent spirals in the single-spiral coil is 40-60 mm.
8. The chiral catalytic device according to any one of claims 3 to 5, wherein the reaction chamber (1) is further communicated with a gas inlet (5); the reaction cavity (1) is also communicated with a raw material pump (6).
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