CN114213342A - Production system and method for preparing 6-amino-1,3-dimethyl uracil - Google Patents
Production system and method for preparing 6-amino-1,3-dimethyl uracil Download PDFInfo
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- CN114213342A CN114213342A CN202111428088.3A CN202111428088A CN114213342A CN 114213342 A CN114213342 A CN 114213342A CN 202111428088 A CN202111428088 A CN 202111428088A CN 114213342 A CN114213342 A CN 114213342A
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- VFGRNTYELNYSKJ-UHFFFAOYSA-N 6-amino-1,3-dimethylpyrimidine-2,4-dione Chemical compound CN1C(N)=CC(=O)N(C)C1=O VFGRNTYELNYSKJ-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 79
- 239000002994 raw material Substances 0.000 claims abstract description 75
- 239000007788 liquid Substances 0.000 claims abstract description 33
- QCTAUOIBRPZHKI-UHFFFAOYSA-N 2-cyano-n-(dimethylcarbamoyl)acetamide Chemical compound CN(C)C(=O)NC(=O)CC#N QCTAUOIBRPZHKI-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003513 alkali Substances 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 13
- 238000009826 distribution Methods 0.000 claims abstract description 9
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000012295 chemical reaction liquid Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 13
- 238000003860 storage Methods 0.000 claims description 12
- 239000012530 fluid Substances 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 27
- 235000011121 sodium hydroxide Nutrition 0.000 abstract description 9
- 239000000047 product Substances 0.000 abstract description 4
- 238000000889 atomisation Methods 0.000 abstract description 3
- GEWLAWPECHTDOX-UHFFFAOYSA-N n-carbamoyl-2-cyano-n-methylacetamide Chemical compound NC(=O)N(C)C(=O)CC#N GEWLAWPECHTDOX-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 1
- 239000013589 supplement Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 description 6
- 238000007363 ring formation reaction Methods 0.000 description 6
- 230000003750 conditioning effect Effects 0.000 description 5
- 238000010924 continuous production Methods 0.000 description 5
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 4
- -1 6-amino-1,3-dimethyl uracil urea Chemical compound 0.000 description 3
- 239000003518 caustics Substances 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229960001948 caffeine Drugs 0.000 description 2
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- ZFXYFBGIUFBOJW-UHFFFAOYSA-N theophylline Chemical compound O=C1N(C)C(=O)N(C)C2=C1NC=N2 ZFXYFBGIUFBOJW-UHFFFAOYSA-N 0.000 description 2
- 229960003556 aminophylline Drugs 0.000 description 1
- FQPFAHBPWDRTLU-UHFFFAOYSA-N aminophylline Chemical compound NCCN.O=C1N(C)C(=O)N(C)C2=C1NC=N2.O=C1N(C)C(=O)N(C)C2=C1NC=N2 FQPFAHBPWDRTLU-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229960000278 theophylline Drugs 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D239/00—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings
- C07D239/02—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings
- C07D239/24—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D239/28—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms
- C07D239/46—Two or more oxygen, sulphur or nitrogen atoms
- C07D239/52—Two oxygen atoms
- C07D239/54—Two oxygen atoms as doubly bound oxygen atoms or as unsubstituted hydroxy radicals
- C07D239/545—Two oxygen atoms as doubly bound oxygen atoms or as unsubstituted hydroxy radicals with other hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The application discloses a production system and a method for preparing 6-amino-1,3-dimethyl uracil. The method comprises the steps of taking a methyl cyanoacetylurea solution and liquid caustic soda as raw materials, inputting the dimethyl cyanoacetylurea solution and the liquid caustic soda into an impinging stream reactor at a certain speed, enabling the dimethyl cyanoacetylurea solution and the liquid caustic soda to be in rapid contact and fully mixed in the reactor, then enabling the mixture to enter a reaction kettle, controlling the temperature of the reaction kettle to be 50-150 ℃, carrying out an on-line pH meter, controlling pH to supplement the liquid caustic soda according to a terminal point, generating 6-amino-1,3-dimethyl uracil slurry in the reaction kettle by the dimethyl cyanoacetylurea solution and the liquid caustic soda, and obtaining a product of 6-amino-1,3-dimethyl uracil after centrifugal separation. In the reaction process, the 6-amino-1,3-dimethyl uracil is prepared by impinging stream atomization reaction, and the particle size distribution can be controlled. In the invention, the liquid alkali and the dimethyl cyanoacetylurea solution are continuously fed, and the two solutions are quickly and uniformly mixed in the impinging stream mixer, so that the reaction efficiency is improved, and good economic efficiency can be obtained.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a production system and a method for preparing 6-amino-1,3-dimethyl uracil.
Background
6-amino-1, 3-dimethyluracils, CAS number: 6642-31-5; molecular formula C6H9N3O2The English name is 6-Amino-1,3-dimethyl-1,2,3,4-tetrahydropyrimidine-2,4-dione, commonly called dimethyl 4AU, the molecular weight is 155.15, the melting point is 295 ℃, and the main application is used for producing caffeine, theophylline, aminophylline raw materials, dye auxiliary agents and the like.
The 6-amino-1,3-dimethyl uracil is an important medicine and coffee intermediate, is a cyclization reaction product in the caffeine technological process, is also a starting material of a cyclization reaction, is used as a connecting link of the cyclization reaction and the cyclization reaction, has good quality, can reflect the cyclization reaction degree, and can control the cyclization reaction from the source of the starting material, so that the yield and the purity of the 6-amino-1,3-dimethyl uracil are improved, and quality guarantee is provided for subsequent reactions.
Patent application No. CN107540618A discloses an invention patent named as 'a preparation method of 6-amino-1,3-dimethyl uracil', but the process method is intermittent operation, and has the disadvantages of large labor capacity, long reaction time and low yield. At present, no patent and article related to the continuous preparation process of 6-amino-1,3-dimethyl uracil is reported. The reason is that the particle size distribution of the 6-amino-1,3-dimethyl uracil cannot be controlled, and the intermittent operation is required, so that the continuous production system and the continuous production method for preparing the 6-amino-1,3-dimethyl uracil are provided, which is a technical problem to be solved.
Disclosure of Invention
The invention aims to provide a production system and a method for preparing 6-amino-1,3-dimethyl uracil, which are used for solving the technical problems that the yield and the purity of 6-amino-1,3-dimethyl uracil cannot be controlled, the particle size distribution of 6-amino-1,3-dimethyl uracil cannot be controlled, continuous production cannot be realized, intermittent operation is adopted, the labor amount is large, the reaction time is long, and the yield is low in the preparation method of 6-amino-1,3-dimethyl uracil in the prior art.
In order to achieve the above objects, one embodiment of the present invention provides a production system for preparing 6-amino-1,3-dimethyl uracil, comprising an impinging stream reactor and a reaction kettle; the side wall of the impinging stream reactor is provided with a first inlet and a second inlet which are correspondingly arranged, and the bottom wall of the impinging stream reactor is provided with an outlet; the first inlet is used for inputting a first raw material solution, the second inlet is used for inputting a second raw material solution, and the first raw material solution and the second raw material solution are fully contacted and mixed in the impinging stream reactor; the reaction kettle is communicated with the outlet of the impinging stream reactor; and a stirrer, a PH regulator and a temperature regulator are arranged in the reaction kettle.
Further, the reaction kettle further comprises a centrifugal separator or the reaction kettle is further connected to a centrifuge.
Further, the production system for preparing 6-amino-1,3-dimethyl uracil also comprises: a first raw material storage tank and a second raw material storage tank; the first raw material storage tank stores a first raw material solution and is communicated with the first inlet through a first pump; the second raw material storage tank stores a second raw material solution and is communicated with the second inlet through a second pump; the first raw material solution and the second raw material solution are not dimethyl cyanoacetylurea solution and liquid alkali solution simultaneously; the first inlet and the second inlet form a nozzle towards the inside of the impinging stream reactor, and the nozzles at the positions of the first inlet and the second inlet are arranged on a straight line.
Further, the PH regulator comprises a PH meter and a regulating liquid supply pump, the PH meter is used for detecting the PH value of the reaction liquid in the reaction kettle after the reaction liquid fully reacts, and the PH meter is electrically connected to the regulating liquid supply pump and used for controlling the opening and closing of the regulating liquid supply pump according to the detected PH value.
The present application also provides a method for preparing 6-amino-1, 3-dimethyluracil comprising the steps of: a raw material solution mixing step, namely taking a dimethyl cyanoacetylurea solution and a liquid alkali solution as a first raw material solution and a second raw material solution, respectively inputting the first raw material solution and the second raw material solution into an impinging stream reactor through a first inlet and a second inlet correspondingly, and fully contacting and mixing the first raw material solution and the second raw material solution in the impinging stream reactor to obtain a reaction solution; a reaction control step, namely, feeding the mixed reaction liquid into a reaction kettle, controlling the temperature in the reaction kettle to ensure that the reaction liquid fully reacts, and adjusting the pH value after the reaction liquid fully reacts to generate 6-amino-1,3-dimethyl uracil slurry; and a centrifugal separation step, wherein the 6-amino-1,3-dimethyl uracil slurry is subjected to centrifugal separation to obtain a product 6-amino-1,3-dimethyl uracil.
Further, in the step of mixing the raw material solutions, the particle size distribution of the 6-amino-1, 3-dimethyluracil in the reaction liquid is controlled by adjusting the fluid pressures and flow rates of the first raw material solution and the second raw material solution supplied at the first inlet and the second inlet of the impinging stream reactor.
Further, in the step of mixing the raw material solution, the mass fraction of the dimethyl cyanoacetylurea solution is 50%, and the mass fraction of the liquid caustic soda solution is 20% -30%.
Further, in the reaction control step, the pH value of the reaction solution in the reaction kettle after the reaction is fully performed is finally adjusted to 9-10.
Further, in the reaction control step, the temperature in the reaction vessel is controlled to 50 to 100 ℃.
Further, in the reaction control step, the reaction equation of the reaction liquid in the reaction vessel is as follows:
the invention has the beneficial effects that the production system and the method for preparing the 6-amino-1,3-dimethyl uracil are provided, the 6-amino-1,3-dimethyl uracil is prepared through impinging stream atomization reaction, and the particle size distribution can be controlled. In the invention, the liquid alkali and the dimethyl cyanoacetylurea solution are continuously fed, and the two solutions are quickly and uniformly mixed in the impinging stream mixer, so that the reaction efficiency is improved, and good economic efficiency can be obtained.
Drawings
The technical solution and other advantages of the present application will be presented in the following detailed description of specific embodiments of the present application with reference to the accompanying drawings.
FIG. 1 is a schematic diagram of a production system for preparing 6-amino-1, 3-dimethyluracil provided in the examples of this application.
FIG. 2 is a flow diagram of a process for preparing 6-amino-1, 3-dimethyluracil provided in the examples herein.
The labels in the figure are as follows:
1-first raw material storage tank, 2-first pump, 3-impinging stream reactor, 4-second raw material storage tank, 5-second pump, 6-regulating liquid supply pump, 7-reaction kettle, 8-pH meter, 9-stirrer, 31-first inlet, 32-second inlet, and 33-outlet.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. It is to be understood that the embodiments described are only a few embodiments of the present application and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
In the description of the present application, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; may be mechanically connected, may be electrically connected or may be in communication with each other; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.
Specifically, referring to fig. 1, the present application provides a production system for preparing 6-amino-1,3-dimethyl uracil, comprising an impinging stream reactor 3 and a reaction kettle 7; the side wall of the impinging stream reactor 3 is provided with a first inlet 31 and a second inlet 32 which are correspondingly arranged, and the bottom wall of the impinging stream reactor is provided with an outlet 33; the first inlet 31 inputs a first raw material solution, the second inlet 32 inputs a second raw material solution, and the first raw material solution and the second raw material solution are fully contacted and mixed in the impinging stream reactor 3; the reaction kettle 7 is communicated with the outlet 33 of the impinging stream reactor 3; and a stirrer 9, a pH regulator and a temperature regulator are arranged in the reaction kettle 7. The stirrer 9 is arranged at the top of the reaction kettle 7, the impeller extends into the cavity of the reaction kettle 7, and the temperature regulator is arranged on the side wall or the bottom wall of the reaction kettle 7.
In the embodiment of the present application, the reaction kettle 7 further comprises a centrifugal separator or the reaction kettle 7 is further connected to a centrifuge.
In the embodiment of the application, the production system for preparing 6-amino-1,3-dimethyl uracil further comprises: a first raw material storage tank 1 and a second raw material storage tank 4; the first raw material storage tank 1 stores a first raw material solution and is communicated with the first inlet 31 through a first pump 2; the second raw material storage tank 4 stores a second raw material solution and is communicated with the second inlet 32 through a second pump 5; the first raw material solution and the second raw material solution are not dimethyl cyanoacetylurea solution and liquid alkali solution simultaneously; the liquid alkali solution is preferably NaOH; the first inlet 31 and the second inlet 32 form a nozzle towards the inside of the impinging stream reactor 3, and the nozzles at the positions of the first inlet 31 and the second inlet 32 are arranged in a straight line. The particle size distribution of the 6-amino-1, 3-dimethyluracil in the reaction liquid is controlled by adjusting the fluid pressure and flow rate of the first feedstock solution and the second feedstock solution supplied from the nozzles at the first inlet 31 and the second inlet 32 of the impinging stream reactor 3. Therefore, the particle size can be effectively controlled, the aggregation and deposition are reduced, and the continuous production is facilitated.
In the embodiment of this application, the PH regulator includes PH meter 8 and regulating solution supply pump 6, PH meter 8 is used for detecting the PH value after the reaction is fully reacted to the reaction liquid in reation kettle 7, PH meter 8 electric connection to regulating solution supply pump 6 is used for according to the PH value control that detects opening and closing of regulating solution supply pump 6. Preferably, the conditioning liquid supply pump 6 is connected to the reservoir of the liquid caustic solution, and when the liquid caustic solution is stored in the first raw material reservoir 1, the conditioning liquid supply pump 6 is connected to the first raw material reservoir 1; when the liquid caustic solution is stored in the second raw material tank 4, the conditioning liquid supply pump 6 is connected to the second raw material tank 4. It will be appreciated that the conditioning fluid supply pump 6 may also be connected separately to an external conditioning fluid reservoir.
Referring to FIG. 2, based on the production system for preparing 6-amino-1, 3-dimethyluracil as described above, the present application also provides a method for preparing 6-amino-1, 3-dimethyluracil, comprising steps S1-S3.
S1, mixing raw material solutions, namely, taking a dimethyl cyanoacetylurea solution and a liquid alkali solution as a first raw material solution and a second raw material solution, respectively and correspondingly inputting the first raw material solution and the second raw material solution into the impinging stream reactor 3 through a first inlet 31 and a second inlet 32, and fully contacting and mixing the first raw material solution and the second raw material solution in the impinging stream reactor 3 to obtain a reaction solution.
S2, a reaction control step, namely, feeding the mixed reaction liquid into a reaction kettle 7, controlling the temperature in the reaction kettle 7 to ensure that the reaction liquid fully reacts, and adjusting the pH value after the reaction liquid fully reacts to generate 6-amino-1,3-dimethyl uracil slurry.
S3, a centrifugal separation step, wherein the 6-amino-1,3-dimethyl uracil slurry is centrifugally separated to obtain a product 6-amino-1,3-dimethyl uracil.
In the present example, in the step S1 of mixing the raw material solution, the particle size distribution of the 6-amino-1, 3-dimethyluracil in the reaction liquid is controlled by adjusting the fluid pressure and flow rate of the first raw material solution and the second raw material solution supplied at the first inlet 31 and the second inlet 32 of the impinging stream reactor 3. Therefore, the particle size can be effectively controlled, the aggregation and deposition are reduced, and the continuous production is facilitated.
In the embodiment of the application, in the step S1 of mixing the raw material solution, the mass fraction of the dimethyl cyanoacetylurea solution is 50%, and the mass fraction of the liquid caustic soda solution is 20% -30%.
In the present embodiment, in the reaction control step S2, the PH of the reaction solution in the reaction kettle 7 after the reaction is completed is finally adjusted to 9 to 10.
In the present embodiment, in the reaction control step S2, the temperature in the reaction kettle 7 is controlled to be 50 to 100 ℃, preferably 80 to 85 ℃.
In the present embodiment, in the reaction control step S2, the liquid alkali solution is preferably NaOH; the reaction equation of the reaction liquid in the reaction kettle 7 is as follows:
the 6-amino-1,3-dimethyl uracil obtained by mixing in the impinging stream reactor 3 and reacting in the reaction kettle 7 is white powder, high in purity, small in particle size and uniform in particle size.
The invention has the beneficial effects that the production system and the method for preparing 6-amino-1,3-dimethyl uracil urea are characterized in that methyl cyanoacetylurea solution and liquid alkali are used as raw materials, the dimethyl cyanoacetylurea solution and the liquid alkali are input into an impinging stream reactor at a certain speed, are rapidly contacted and fully mixed in the reactor, then enter a reaction kettle, the temperature of the reaction kettle is controlled to be 50-150 ℃, an online pH meter is arranged, the liquid alkali is replenished according to the end point control pH, the dimethyl cyanoacetylurea solution and the liquid alkali generate 6-amino-1,3-dimethyl uracil urea slurry in the reaction kettle, and the product 6-amino-1,3-dimethyl uracil urea is obtained after centrifugal separation. In the reaction process, the 6-amino-1,3-dimethyl uracil is prepared by impinging stream atomization reaction, and the particle size distribution can be controlled. In the invention, the liquid alkali and the dimethyl cyanoacetylurea solution are continuously fed, and the two solutions are quickly and uniformly mixed in the impinging stream mixer, so that the reaction efficiency is improved, and good economic efficiency can be obtained.
In the foregoing embodiments, the descriptions of the respective embodiments have respective emphasis, and for parts that are not described in detail in a certain embodiment, reference may be made to related descriptions of other embodiments.
The above embodiments of the present application are described in detail, and specific examples are applied in the present application to explain the principles and implementations of the present application, and the description of the above embodiments is only used to help understand the technical solutions and core ideas of the present application; those of ordinary skill in the art will understand that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications or substitutions do not depart from the spirit and scope of the present disclosure as defined by the appended claims.
Claims (10)
1. A production system for preparing 6-amino-1, 3-dimethyluracil, comprising:
the side wall of the impinging stream reactor is provided with a first inlet and a second inlet which are correspondingly arranged, and the bottom wall of the impinging stream reactor is provided with an outlet; the first inlet is used for inputting a first raw material solution, the second inlet is used for inputting a second raw material solution, and the first raw material solution and the second raw material solution are fully contacted and mixed in the impinging stream reactor; and
the reaction kettle is communicated with the outlet of the impinging stream reactor; and a stirrer, a PH regulator and a temperature regulator are arranged in the reaction kettle.
2. The production system for producing 6-amino-1, 3-dimethyluracil according to claim 1, wherein the reaction tank further comprises a centrifugal separator or the reaction tank is further connected to a centrifuge.
3. The production system for 6-amino-1, 3-dimethyluracil according to claim 1, further comprising:
the first raw material storage tank stores a first raw material solution and is communicated with the first inlet through a first pump; and
the second raw material storage tank is used for storing a second raw material solution and is communicated with the second inlet through a second pump;
the first raw material solution and the second raw material solution are not dimethyl cyanoacetylurea solution and liquid alkali solution simultaneously; the first inlet and the second inlet form a nozzle towards the inside of the impinging stream reactor, and the nozzles at the positions of the first inlet and the second inlet are arranged on a straight line.
4. The system for preparing 6-amino-1, 3-dimethyluracil as set forth in claim 1, wherein the pH controller comprises a pH meter for detecting a pH value of the reaction solution in the reaction vessel after the reaction solution has been sufficiently reacted, and a control solution supply pump electrically connected to the pH meter for controlling the control of the control solution supply pump to be turned on and off according to the detected pH value.
5. A process for preparing 6-amino-1, 3-dimethyluracil comprising the steps of:
a raw material solution mixing step, namely taking a dimethyl cyanoacetylurea solution and a liquid alkali solution as a first raw material solution and a second raw material solution, respectively inputting the first raw material solution and the second raw material solution into an impinging stream reactor through a first inlet and a second inlet correspondingly, and fully contacting and mixing the first raw material solution and the second raw material solution in the impinging stream reactor to obtain a reaction solution;
a reaction control step, namely, feeding the mixed reaction liquid into a reaction kettle, controlling the temperature in the reaction kettle to ensure that the reaction liquid fully reacts, and adjusting the pH value after the reaction liquid fully reacts to generate 6-amino-1,3-dimethyl uracil slurry; and
and (3) a centrifugal separation step, wherein the 6-amino-1,3-dimethyl uracil slurry is subjected to centrifugal separation to obtain a product 6-amino-1,3-dimethyl uracil.
6. The method of claim 5, wherein the particle size distribution of 6-amino-1, 3-dimethyluracil in the reaction solution is controlled by adjusting the fluid pressure and flow rate of the first and second raw material solutions supplied at the first and second inlets of the impinging stream reactor during the step of mixing the raw material solutions.
7. The method for preparing 6-amino-1, 3-dimethyluracil as described in claim 5, wherein the dimethylcyanoacetylurea solution is 50% by mass and the liquid alkali solution is 20% to 30% by mass in the step of mixing the raw material solutions.
8. The method for producing 6-amino-1, 3-dimethyluracil according to claim 5, wherein the pH of the reaction solution in the reaction vessel after the reaction is sufficiently carried out is finally adjusted to 9 to 10 in the reaction control step.
9. The method for producing 6-amino-1, 3-dimethyluracil according to claim 5, wherein the temperature in the reaction vessel is controlled to 50 to 100 ℃ in the reaction control step.
10. The method for producing 6-amino-1, 3-dimethyluracil according to claim 5, wherein in the reaction control step, the reaction equation of the reaction liquid in the reaction tank is as follows:
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| CN115260106A (en) * | 2022-09-23 | 2022-11-01 | 新华制药（寿光）有限公司 | Preparation method of 6-amino-1, 3-dimethyl uracil |
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