CN115960107A - Method for synthesizing TAIW through continuous hydrogenation and debenzylation based on microchannel reactor - Google Patents
Method for synthesizing TAIW through continuous hydrogenation and debenzylation based on microchannel reactor Download PDFInfo
- Publication number
- CN115960107A CN115960107A CN202211653790.4A CN202211653790A CN115960107A CN 115960107 A CN115960107 A CN 115960107A CN 202211653790 A CN202211653790 A CN 202211653790A CN 115960107 A CN115960107 A CN 115960107A
- Authority
- CN
- China
- Prior art keywords
- taiw
- microchannel reactor
- synthesizing
- gas
- continuous
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 29
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 18
- 238000006264 debenzylation reaction Methods 0.000 title claims abstract description 10
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 35
- 239000012530 fluid Substances 0.000 claims abstract description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 15
- 239000001257 hydrogen Substances 0.000 claims abstract description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011949 solid catalyst Substances 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- 239000003054 catalyst Substances 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 17
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 15
- 229910052763 palladium Inorganic materials 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 8
- 235000019253 formic acid Nutrition 0.000 claims description 8
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 230000014759 maintenance of location Effects 0.000 claims description 4
- NXJCBFBQEVOTOW-UHFFFAOYSA-L palladium(2+);dihydroxide Chemical compound O[Pd]O NXJCBFBQEVOTOW-UHFFFAOYSA-L 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 239000012263 liquid product Substances 0.000 claims description 2
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 claims description 2
- 235000011054 acetic acid Nutrition 0.000 claims 1
- 235000019441 ethanol Nutrition 0.000 claims 1
- 235000019439 ethyl acetate Nutrition 0.000 claims 1
- 229910003445 palladium oxide Inorganic materials 0.000 claims 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims 1
- 229910052814 silicon oxide Inorganic materials 0.000 claims 1
- 238000000746 purification Methods 0.000 abstract description 2
- HVYHGOIMTRVUCH-UHFFFAOYSA-N molport-002-842-999 Chemical compound CC(=O)N1C2NC3N(C(C)=O)C4C1N(C(C)=O)C2NC3N4C(C)=O HVYHGOIMTRVUCH-UHFFFAOYSA-N 0.000 description 19
- 239000000047 product Substances 0.000 description 13
- 239000000243 solution Substances 0.000 description 12
- 230000008569 process Effects 0.000 description 10
- NDYLCHGXSQOGMS-UHFFFAOYSA-N CL-20 Chemical compound [O-][N+](=O)N1C2N([N+]([O-])=O)C3N([N+](=O)[O-])C2N([N+]([O-])=O)C2N([N+]([O-])=O)C3N([N+]([O-])=O)C21 NDYLCHGXSQOGMS-UHFFFAOYSA-N 0.000 description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 150000002431 hydrogen Chemical class 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 6
- 238000005191 phase separation Methods 0.000 description 6
- 230000006872 improvement Effects 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 238000013375 chromatographic separation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- NINQAYBICGTGQD-UHFFFAOYSA-N 1-(6,8,12-triacetyl-4,10-dibenzyl-2,4,6,8,10,12-hexazatetracyclo[5.5.0.03,11.05,9]dodecan-2-yl)ethanone Chemical compound CC(=O)N1C2C(N3CC=4C=CC=CC=4)N(C(=O)C)C1C(N1C(C)=O)N(C(C)=O)C3C1N2CC1=CC=CC=C1 NINQAYBICGTGQD-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- ZWWCURLKEXEFQT-UHFFFAOYSA-N dinitrogen pentaoxide Chemical compound [O-][N+](=O)O[N+]([O-])=O ZWWCURLKEXEFQT-UHFFFAOYSA-N 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical compound C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 description 2
- 229910052680 mordenite Inorganic materials 0.000 description 2
- 238000006396 nitration reaction Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000009904 heterogeneous catalytic hydrogenation reaction Methods 0.000 description 1
- 238000007327 hydrogenolysis reaction Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- FPLYNRPOIZEADP-UHFFFAOYSA-N octylsilane Chemical group CCCCCCCC[SiH3] FPLYNRPOIZEADP-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a method for synthesizing TAIW by continuous hydrogenation and debenzylation based on a microchannel reactor, which is characterized in that TADBIW is dissolved in an organic solvent to prepare a solution with a certain concentration, the solution is fully mixed with hydrogen in a microchannel reactor to obtain a gas-liquid mixed fluid, the gas-liquid mixed fluid is subjected to continuous hydrogenation and debenzylation reaction by the microchannel reactor filled with a solid catalyst, and the reacted gas-liquid mixture is subjected to gas-liquid separation and purification to obtain a target product TAIW.
Description
Technical Field
The invention belongs to the technical field of fine chemical engineering, and particularly relates to a method for synthesizing TAIWIB by continuous hydrogenation and debenzylation based on a microchannel reactor.
Background
Hexanitrohexaazaisowurtzitane (HNIW) is an energetic material, and Tetraacetylhexaazaisowurtzitane (TAIW) is an important precursor for the synthesis of HNIW. Under the action of a palladium (Pd) catalyst, tetraacetyldibenzylhexaazaisowurtzitane (TADBIw) is subjected to hydrogenolysis debenzylation reaction in an organic solvent medium at a certain temperature and pressure to generate TAIW. Generally, the reported TADBIW hydrodebenzylation reaction mainly adopts a kettle batch synthesis process, and as the reactor needs to be subjected to operations such as multiple times of replacement, hydrogen supplement, temperature rise, temperature reduction and the like in the production process, a large potential safety hazard may exist in large-scale production; in addition, the consumption of the palladium catalyst is large, the production cost is high, and the catalyst is easy to wear and the loss of active species palladium is easy to cause serious reduction of the catalytic performance of the catalyst under the existing reaction process condition due to long-time stirring and mixing. The micro-reactor has the advantages of high mixing efficiency, good mass transfer and heat transfer performance, prolonged service life of the catalyst, good safety and the like, can effectively solve the serious defects of batch intermittent synthesis process of the hydrogenation reaction kettle, improves the production efficiency, reduces the production cost, improves the safety of the synthesis reaction process, realizes the accurate control of the process conditions and ensures the product quality.
The patents related to TAIW synthesized by TADBIW through hydrogenation and debenzylation disclosed in China currently mainly include CN114573595A and CN103288839A. CN114573595A discloses a method for synthesizing CL-20 by catalytic nitration of mordenite, which utilizes the acid sites of the mordenite as a catalyst for synthesizing CL-20 by nitration of tetraacetylhexaazaisowurtzitane in a dinitrogen pentoxide/nitric acid system. The invention of CN103288839A relates to a chromatographic separation method and a quantitative detection method of CL-20 and three intermediates thereof, and discloses a chromatographic separation method and a quantitative detection method of CL-20 and three intermediates thereof. The packing of the chromatographic column used in the disclosed chromatographic separation method is octyl silane bonded silica gel, the mobile phase is a mixed solution of aqueous formic acid and acetonitrile, and the volume ratio of the aqueous formic acid to the acetonitrile is (20-25): (75-80), wherein the volume ratio of formic acid to water in the formic acid aqueous solution is as follows: (0.1-0.4) 100.
The process for synthesizing TAIW by using the continuous hydrogenation and debenzylation of the microchannel reactor is not disclosed in the patent.
Disclosure of Invention
In order to solve the problems, the invention discloses a method for synthesizing TAIW by continuous hydrodebenzylation based on a microchannel reactor, TADBIW is dissolved by a proper amount of solvent to form a mixed solution, the mixed solution is mixed with hydrogen according to a certain proportion and then continuously enters the microchannel reactor filled with a palladium catalyst, the TADBIW generates heterogeneous hydrodebenzylation reaction under the action of the catalyst, and after gas-liquid separation, liquid is separated and purified to obtain TAIW solid.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for synthesizing TAIW by continuous hydrodebenzyl based on a microchannel reactor comprises the following steps:
(1) Dissolving TADBIW in one or more organic solvents selected from alcohol, acid and ester to obtain a mixed solution with a certain concentration;
(2) Mixing the mixed solution obtained in the step (1) with hydrogen in a micro mixer to form gas-liquid mixed fluid;
(3) Carrying out a hydrodebenzylation reaction on the gas-liquid mixed fluid obtained in the step (2) at a certain temperature, pressure and retention time by using a microchannel reactor filled with a solid catalyst;
(4) And (4) carrying out gas-liquid separation on the gas-liquid mixture obtained in the step (3), allowing hydrogen to enter a tail gas treatment system, and separating and purifying a liquid product to obtain TAIW.
As an improvement of the invention, the micromixer in the step (1) is one or a combination of an active mixer and a driven mixer; preferably, the micromixer comprises a membrane dispersion reactor, a micromesh reactor, a T-type reactor, or other micromixers or combinations thereof that enable mixing of the system.
As an improvement of the invention, the microchannel reactor in the step (2) is one or a combination of more than two of a packed bed microreactor, a structural catalyst reactor and a wall-supported catalyst reactor, the diameter of the microchannel is 100 micrometers-50 millimeters, and the length-diameter ratio L/D is more than 1000.
In a modification of the present invention, the organic solvent in step (1) is one or a combination of two or more of methanol, ethanol, formic acid, acetic acid and ethyl acetate.
As an improvement of the invention, the solute mass concentration of the mixed solution in the step (1) is 0.1-25 wt%.
As a modification of the invention, the molar ratio of hydrogen to TADBIW in the step (2) is 0.1 to 20.
As an improvement of the invention, in the step (3), the solid catalyst is any one of palladium hydroxide/carbon, palladium acetate/carbon, palladium/alumina and palladium/silica, and the content of palladium in the solid catalyst is 1-25%.
As an improvement of the invention, in the step (3), the temperature of the hydrogenation and debenzylation reaction is 10-120 ℃, the reaction pressure is 0.1-2.5 MPa, and the retention time is 10-150 s.
The invention has the beneficial effects that:
the method for synthesizing TAIW by continuous hydrogenation and debenzylation based on the microchannel reactor can effectively improve the mass transfer efficiency between gas, liquid and solid in the heterogeneous hydrogenation reaction process of reaction materials, improve the heat transfer capacity of the reactor and reduce the loss of a catalyst; meanwhile, the safety problem of the hydrodebenzylation reaction in the batch synthesis process of the kettle can be solved, the process safety of the reaction is improved, and the accurate control of the process conditions is realized.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a schematic view of a microchannel reactor assembly according to the present invention.
FIG. 3 is a pictorial view of a microchannel reactor assembly of the present invention.
List of reference symbols:
1. the device comprises a raw material dissolving kettle, 2, a filter, 3, a micro-channel reactor, 4, a gas-liquid micro-mixer, 5 and a gas-liquid separator.
Detailed Description
The present invention will be further illustrated with reference to the accompanying drawings and specific embodiments, which are to be understood as merely illustrative of the invention and not as limiting the scope of the invention.
Example 1
(1) Preparing an acetic acid solution of TADBIW, wherein the concentration of TADBIW is 5wt%.
(2) Filtering the mixed solution obtained in the step (1), and then mixing with hydrogen H 2 And mixing in a gas-liquid micro mixer to form gas-liquid mixed fluid.
(3) Passing the gas-liquid mixed fluid obtained in the step (2) through a microchannel reactor packed with a palladium/carbon catalyst (10 wt% Pd) 2 The molar ratio of TADBIW to TADBIW is 15, the reaction temperature is 55 ℃, the pressure is 0.5 MPa, the residence time is controlled to be 120 s, gas-liquid phase separation is carried out at the outlet of the micro packed bed, and the obtained solution is separated and purified to obtain the target product TAIWIB.
After analysis, the conversion rate of TADBIW is 100%, and the yield of TAIW product is 96.8%.
Example 2
(1) A formic acid/methanol solution of TADBIW is prepared, wherein the concentration of TADBIW is 0.1 wt%.
(2) Filtering the mixed solution obtained in the step (1), and then mixing with hydrogen H 2 And mixing in a gas-liquid micromixer to form gas-liquid mixed fluid.
(3) Passing the gas-liquid mixed fluid obtained in the step (2) through a microchannel reactor packed with a palladium hydroxide/carbon catalyst (10 wt% Pd) 2 The molar ratio of TADBIW to TADBIW is 8:1, the reaction temperature is 50 ℃, the pressure is 1.5MPa, the residence time is controlled to be 120 s, gas-liquid phase separation is carried out at the outlet of the micro packed bed, and the obtained solution is separated and purified to obtain the target product TAIWIB.
After analysis, the conversion rate of TADBIW is 100%, and the yield of TAIW product is 97.6%.
Example 3
(1) Preparing an acetic acid solution of TADBIW, wherein the concentration of TADBIW is 5wt%.
(2) Filtering the mixed solution obtained in the step (1), and then mixing with hydrogen H 2 And mixing in a gas-liquid micromixer to form gas-liquid mixed fluid.
(3) Passing the gas-liquid mixed fluid obtained in the step (2) through a microchannel reactor packed with a palladium/carbon catalyst (10 wt% Pd) 2 The molar ratio of TADBIW to TADBIW is 10, the reaction temperature is 50 ℃, the pressure is 1.0MPa, the residence time is controlled to be 100 s, gas-liquid phase separation is carried out at the outlet of the micro packed bed, and the obtained solution is separated and purified to obtain the target product TAIWIB.
After analysis test calculation, the conversion rate of the raw material TADBIW is 100%, and the yield of the TAIW product is 95.2%.
Example 4
(1) An acetic/formic acid solution of TADBIW was prepared with a TADBIW concentration of 10 wt%.
(2) Filtering the mixed solution obtained in the step (1), and then mixing with hydrogen H 2 And mixing in a gas-liquid micromixer to form gas-liquid mixed fluid.
(3) Passing the gas-liquid mixed fluid obtained in the step (2) through a microchannel reactor packed with a palladium-carbon catalyst (10 wt% Pd) 2 The molar ratio of the TADBIW and TADBIW is 5:1, the reaction temperature is 70 ℃, the pressure is 3.0MPa, the residence time is controlled to be 10 s, gas-liquid phase separation is carried out at the outlet of the micro packed bed, and the obtained solution is separated and purified to obtain the target product TAIW.
After analysis, the conversion rate of TADBIW is 100%, and the yield of TAIW product is 96.4%.
Example 5
(1) Preparing an acetic acid solution of TADBIW, wherein the concentration of TADBIW is 15 wt%.
(2) Filtering the mixed solution obtained in the step (1), and mixing with hydrogen H 2 Mixing in a gas-liquid micromixer to form a gas-liquid mixed fluid。
(3) Passing the gas-liquid mixed fluid obtained in the step (2) through a microchannel reactor packed with a palladium-carbon catalyst (6 wt% Pd) 2 The molar ratio of TADBIW to TADBIW is 5:1, the reaction temperature is 70 ℃, the pressure is 2.0MPa, the residence time is controlled to be 60 s, gas-liquid phase separation is carried out at the outlet of a micro packed bed, and the target product TAIWIB is obtained after separation and purification of the obtained solution.
After analysis, the conversion rate of TADBIW is 100%, and the yield of TAIW product is 95.4%.
Example 6
(1) Preparing an acetic acid/ethanol solution of TADBIW, wherein the concentration of TADBIW is 15 wt%.
(2) Filtering the mixed solution obtained in the step (1), and then mixing with hydrogen H 2 And mixing in a gas-liquid micromixer to form gas-liquid mixed fluid.
(3) Passing the gas-liquid mixed fluid obtained in the step (2) through a microchannel reactor packed with a palladium hydroxide/carbon catalyst (20 wt% Pd) 2 The molar ratio of TADBIW to TADBIW is 20, the reaction temperature is 90 ℃, the pressure is 2.0MPa, the residence time is controlled to be 60 s, gas-liquid phase separation is carried out at the outlet of the micro packed bed, and the obtained solution is separated and purified to obtain the target product TAIWIB.
After analysis test calculation, the conversion rate of the raw material TADBIW is 100%, and the yield of the TAIW product is 95.1%.
It should be noted that the above-mentioned embodiments illustrate only preferred embodiments of the invention, and are not intended to limit the scope of the invention, and that those skilled in the art will be able to make modifications and alterations to the above-mentioned embodiments without departing from the spirit of the invention, and such modifications and alterations are intended to be within the scope of the appended claims.
Claims (8)
1. A method for synthesizing TAIW by continuous hydrodebenzyl based on a microchannel reactor is characterized by comprising the following steps:
(1) Dissolving TADBIW in one or more organic solvents selected from alcohol, acid and ester to obtain a mixed solution with a certain concentration;
(2) Mixing the mixed solution obtained in the step (1) with hydrogen in a micro mixer to form gas-liquid mixed fluid;
(3) Carrying out a hydrodebenzylation reaction on the gas-liquid mixed fluid obtained in the step (2) at a certain temperature, pressure and retention time by using a microchannel reactor filled with a solid catalyst;
(4) And (4) carrying out gas-liquid separation on the gas-liquid mixture obtained in the step (3), introducing hydrogen into a tail gas treatment system, and separating and purifying a liquid product to obtain TAIW.
2. The method for synthesizing TAIW through continuous hydrodebenzyl based on the microchannel reactor as recited in claim 1, wherein: the micro mixer in the step (1) is one or a combination of an active mixer and a driven mixer.
3. The method for synthesizing TAIW by continuous hydrodebenzylation based on a microchannel reactor as claimed in claim 1, wherein: the microchannel reactor in the step (2) is one or a combination of more than two of a packed bed microreactor, a structural catalyst reactor and a wall-loaded catalyst reactor, the diameter of the microchannel is 100 micrometers-50 millimeters, and the length-diameter ratio L/D is more than 1000.
4. The method for synthesizing TAIW by continuous hydrodebenzylation based on a microchannel reactor as claimed in claim 1, wherein: the organic solvent in the step (1) is one or the combination of more than two of methanol, ethanol, formic acid, acetic acid and acetic ester.
5. The method for synthesizing TAIW through continuous hydrodebenzyl based on the microchannel reactor as recited in claim 1, wherein: the mass concentration of the solute of the mixed solution in the step (1) is 0.1-25 wt%.
6. The method for synthesizing TAIW through continuous hydrodebenzyl based on the microchannel reactor as recited in claim 1, wherein: the molar ratio of the hydrogen to the TADBIW in the step (2) is 0.1 to 20.
7. The method for synthesizing TAIW by continuous hydrodebenzylation based on a microchannel reactor as claimed in claim 1, wherein: the solid catalyst in the step (3) is any one of palladium hydroxide/carbon, palladium acetate/carbon, palladium chloride/palladium, palladium/alumina and palladium/silicon oxide, and the content of palladium in the solid catalyst is 1-25%.
8. The method for synthesizing TAIW by continuous hydrodebenzylation based on a microchannel reactor as claimed in claim 1, wherein: in the step (3), the temperature of the hydrogenation and debenzylation reaction is 10-120 ℃, the reaction pressure is 0.1MPa-2.5 MPa, and the retention time is 10-150 s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211653790.4A CN115960107A (en) | 2022-12-22 | 2022-12-22 | Method for synthesizing TAIW through continuous hydrogenation and debenzylation based on microchannel reactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211653790.4A CN115960107A (en) | 2022-12-22 | 2022-12-22 | Method for synthesizing TAIW through continuous hydrogenation and debenzylation based on microchannel reactor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115960107A true CN115960107A (en) | 2023-04-14 |
Family
ID=87362698
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211653790.4A Pending CN115960107A (en) | 2022-12-22 | 2022-12-22 | Method for synthesizing TAIW through continuous hydrogenation and debenzylation based on microchannel reactor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115960107A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115093409A (en) * | 2022-06-11 | 2022-09-23 | 河南新天地药业股份有限公司 | Method for synthesizing moxifloxacin side chain by continuous hydrodebenzylation in microreactor |
-
2022
- 2022-12-22 CN CN202211653790.4A patent/CN115960107A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115093409A (en) * | 2022-06-11 | 2022-09-23 | 河南新天地药业股份有限公司 | Method for synthesizing moxifloxacin side chain by continuous hydrodebenzylation in microreactor |
Non-Patent Citations (1)
| Title |
|---|
| 唐晓飞等: "钯催化TADBIW氢解合成TAIW", 《应用化工》, vol. 51, no. 11, pages 3163 - 225 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112979583B (en) | Method for synthesizing piperidine by continuous liquid-phase hydrogenation of pyridine in microreactor | |
| CN113402395B (en) | Method for continuously and efficiently synthesizing m-phenylenediamine based on fixed bed microreactor | |
| CN113563201B (en) | Method for continuously and efficiently synthesizing 3, 4-dichloroaniline based on fixed bed microreactor | |
| CN113429295B (en) | Method for preparing m-phenylenediamine by continuous catalytic hydrogenation based on fixed bed microreactor | |
| CN112341395B (en) | Micro-reaction system and method for continuously preparing 2-methyl-4-amino-5-aminomethyl pyrimidine by using same | |
| CN110627650B (en) | Device for continuously synthesizing benzylamine substances through heterogeneous hydrogenation in microreactor | |
| CN107628929B (en) | Production process for preparing 1, 2-propylene glycol by glycerol hydrogenolysis | |
| CN116947795B (en) | Continuous synthesis method of S-hydroxypropyl tetrahydropyran triol | |
| CN104402687B (en) | A kind of production technique of phenol hydrogenation preparing cyclohexanone | |
| CN102070488A (en) | Method for preparing ketoxime | |
| CN115960107A (en) | Method for synthesizing TAIW through continuous hydrogenation and debenzylation based on microchannel reactor | |
| CN107619374A (en) | A kind of method for continuously synthesizing of p-phenylenediamine | |
| CN114394937B (en) | Method for synthesizing 1, 3-dimethyl-2-imidazolone by one-step continuous hydrogenation based on fixed bed microreactor | |
| CN110229074A (en) | A kind of preparation method of N- benzyloxycarbonyl group -2- amino -1- propyl alcohol | |
| CN103709010B (en) | A kind of by tetrahydrobenzene, carboxylic acid and water Reactive Synthesis hexalin method | |
| CN113584099B (en) | Method for preparing dihydrocoumarin or derivative thereof by adopting micro-flow field reaction technology | |
| CN115093409A (en) | Method for synthesizing moxifloxacin side chain by continuous hydrodebenzylation in microreactor | |
| CN109438175B (en) | Method for preparing cyclohexanol and cyclohexanone by decomposing cyclohexyl hydroperoxide | |
| CN114516812A (en) | Full continuous flow preparation method of levocarnitine | |
| CN113527126A (en) | Method for synthesizing 3-nitro-4-methoxyacetanilide by continuous flow microchannel reactor | |
| CN113200875B (en) | Micro-reaction system and method for continuously preparing 2-amino-1, 3-diol compound | |
| CN216024770U (en) | Device for preparing p-trifluoromethoxyaniline through continuous catalytic hydrogenation | |
| CN102872893A (en) | Catalyst used in process of preparing anhydrous formaldehyde by methanol dehydrogenation and preparation method and application process of catalyst | |
| CN112457163B (en) | Micro-channel mixed catalytic hydrogenation device and method for preparing isophorol | |
| CN117586111B (en) | Method for preparing tetrahydrocurcumin through continuous catalytic hydrogenation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |