CN107663162B - A kind of13C-urea synthesis control method - Google Patents
A kind of13C-urea synthesis control method Download PDFInfo
- Publication number
- CN107663162B CN107663162B CN201610599129.8A CN201610599129A CN107663162B CN 107663162 B CN107663162 B CN 107663162B CN 201610599129 A CN201610599129 A CN 201610599129A CN 107663162 B CN107663162 B CN 107663162B
- Authority
- CN
- China
- Prior art keywords
- reaction kettle
- pressure
- urea synthesis
- reaction
- urea
- 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.)
- Active
Links
- 239000004202 carbamide Substances 0.000 title claims abstract description 71
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 48
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 92
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 32
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 5
- 239000011593 sulfur Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 12
- 239000001307 helium Substances 0.000 claims description 9
- 229910052734 helium Inorganic materials 0.000 claims description 9
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 9
- 239000000523 sample Substances 0.000 claims description 9
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 8
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 8
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 6
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 6
- 239000002912 waste gas Substances 0.000 claims description 6
- 238000010926 purge Methods 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 3
- 238000000746 purification Methods 0.000 claims 1
- 239000007789 gas Substances 0.000 abstract description 20
- 238000002360 preparation method Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 3
- WHBHBVVOGNECLV-OBQKJFGGSA-N 11-deoxycortisol Chemical compound O=C1CC[C@]2(C)[C@H]3CC[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 WHBHBVVOGNECLV-OBQKJFGGSA-N 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 13
- 229910052799 carbon Inorganic materials 0.000 description 13
- 241000590002 Helicobacter pylori Species 0.000 description 6
- 229940037467 helicobacter pylori Drugs 0.000 description 6
- XSQUKJJJFZCRTK-OUBTZVSYSA-N Urea-13C Chemical compound N[13C](N)=O XSQUKJJJFZCRTK-OUBTZVSYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 2
- 208000018522 Gastrointestinal disease Diseases 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 208000010643 digestive system disease Diseases 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 208000018685 gastrointestinal system disease Diseases 0.000 description 2
- 208000015181 infectious disease Diseases 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 241001522296 Erithacus rubecula Species 0.000 description 1
- 208000007882 Gastritis Diseases 0.000 description 1
- 208000005577 Gastroenteritis Diseases 0.000 description 1
- 206010019375 Helicobacter infections Diseases 0.000 description 1
- 208000005718 Stomach Neoplasms Diseases 0.000 description 1
- 208000007107 Stomach Ulcer Diseases 0.000 description 1
- 108010046334 Urease Proteins 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 208000000718 duodenal ulcer Diseases 0.000 description 1
- 201000006549 dyspepsia Diseases 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 206010017758 gastric cancer Diseases 0.000 description 1
- 201000005917 gastric ulcer Diseases 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 231100000206 health hazard Toxicity 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000001575 pathological effect Effects 0.000 description 1
- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
- 238000012134 rapid urease test Methods 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 201000011549 stomach cancer Diseases 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
- C07C273/02—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B59/00—Introduction of isotopes of elements into organic compounds ; Labelled organic compounds per se
- C07B59/001—Acyclic or carbocyclic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/05—Isotopically modified compounds, e.g. labelled
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a13The C-urea synthesis control method comprises the following steps: s100, filling raw materials: weighing methanol and sulfur, putting into a reaction kettle, cooling the reaction kettle by using liquid nitrogen, and sequentially communicating13CO and NH3To finish13CO and NH3Filling the liquefied mixture into a reaction kettle; s200, urea synthesis reaction: and sealing the reaction kettle, controlling the temperature to be 80-120 ℃, and detecting the pressure value in the reaction kettle until the pressure in the reaction kettle is reduced to be constant, so that the reaction is finished. The invention uses cooling technology to fill raw material gas in the pressure-resistant reaction kettle, so that the liquid state in the reaction system is realized13CO、NH3And solid simple substance S are synthesized in a pressure-resistant reaction kettle13C-urea, so that the temperature and pressure conditions in the reaction kettle reach the required conditions for urea synthesis, and the realization13And (3) large-scale preparation of the C-urea.
Description
Technical Field
The invention relates to a chemical synthesis method, in particular to a method for synthesizing a synthetic material13A C-urea synthesis control method.
Background
Helicobacter pylori (Hp), a unipolar, multiflagellated, blunt-ended, helically-curved bacterium, was first discovered in 1982 by Barry marshall (Barry j. marshall) and robin warren (j. robinwarren), both of which thus received the 2005 nobel prize in physiology or medicine. Subsequent studies have confirmed that this bacterium does cause gastritis, chronic gastroenteritis, gastric ulcer, duodenal ulcer, non-ulcer dyspepsia and partial gastric cancer, helicobacter pylori has therefore received attention from the medical community, and the relationship between helicobacter pylori infection and gastrointestinal disease has been a hot spot and difficulty in global gastrointestinal disease infection studies for over 30 years.
The current methods for detecting and identifying helicobacter pylori (Hp) mainly comprise a rapid urease test, a helicobacter pylori (Hp) antibody test,13C or14C, expiration test, pathological tissue section, bacterial culture and the like. Wherein,13c or14C, the accuracy of the breath test is the highest and reaches more than 95-96%.13The C-urea is produced13The C breath test detection reagent needs raw material medicines, and the scale preparation technology and the process thereof have difficulties.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provide a13A C-urea synthesis control method, which solves the problem that the prior art can not prepare in large scale13C-problem of urea.
In order to solve the problems, the invention provides the following technical scheme: provide a13The C-urea synthesis control method comprises the following steps:
s100, filling raw materials: weighing methanol and sulfur, putting into a reaction kettle, cooling the reaction kettle by using liquid nitrogen, and sequentially communicating13CO and NH3To finish13CO and NH3Filling the liquefied mixture into a reaction kettle;
s200, urea synthesis reaction: and sealing the reaction kettle, controlling the temperature to be 80-120 ℃, and detecting the pressure value in the reaction kettle until the pressure in the reaction kettle is reduced to be constant, so that the reaction is finished.
In the invention provided13In the C-urea synthesis control method, the step S100 is preceded by the step of:
s010, purging a reaction kettle: helium was used to evacuate the air from the autoclave.
In the invention provided13In the C-urea synthesis control method, in the step S010, helium output pressure is greater than pressure in the reaction kettle; the output pressure of helium is 10-15 psig, and the pressure in the reaction kettle is 0-5 psig.
In the invention provided13In the C-urea synthesis control method, in the step S100, the temperature range in the reaction kettle is-160 to-200 ℃, and the pressure is-14 to-10 psig;13the filling stage of the CO is carried out,13the CO output pressure is 30-100 psig; NH (NH)3Filling stage, NH3The output pressure is 50-200 psig.
In the invention provided13In the C-urea synthesis control method, in the step S200, the pressure in the reaction kettle is gradually reduced along with the urea synthesis reaction; the pressure in the reaction kettle is less than 1500psig when the urea synthesis reaction is just started, and the pressure in the reaction kettle is 100-200 psig when the urea synthesis reaction is completed.
In the invention provided13In the C-urea synthesis control method, the step S200 is followed by the step of:
s300, waste gas removal: and (3) exhausting residual waste gas in the reaction kettle after the urea synthesis reaction is finished by using nitrogen.
In the invention provided13In the C-urea synthesis control method, in the step S300, the output pressure of nitrogen is greater than the pressure in the reaction kettle; the output pressure of the nitrogen source is 10-15 psig, and the pressure in the reaction kettle is 0-5 psig.
In the invention provided13The C-urea synthesis control method also comprises a gas leakage monitoring step: in the urea synthesis process, an air draft device is used for keeping the operating room at negative pressure; an ammonia gas sensing probe, a carbon monoxide sensing probe and a hydrogen sulfide sensing probe are respectively arranged in the operation room and the air exhaust pipeline, and when the content of ammonia gas and/or carbon monoxide and/or hydrogen sulfide exceeds a preset value, the system gives an alarm.
In the invention provided13In the C-urea synthesis control method, the reaction kettle can resist 3000psig pressure.
In the invention provided13In the control method for synthesizing the C-urea,generated by13The C-urea is purified to obtain a pure product with the purity of over 99 percent.
The implementation of the invention has the following beneficial effects: the raw material gas is filled in a pressure-resistant reaction kettle by using a cooling technology, so that the reaction system is in a liquid state13CO、NH3And solid simple substance S are synthesized in a pressure-resistant reaction kettle13C-urea, so that the temperature and pressure conditions in the reaction kettle reach the required conditions for urea synthesis, and the realization13And (3) large-scale preparation of the C-urea.
Drawings
The invention will be further described with reference to the accompanying drawings and examples, in which:
FIG. 1 is a drawing of the present invention13A flow chart of a preferred embodiment of the C-urea synthesis control method.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
13The main component of the breath test reagent used in the C breath test is13C-urea, i.e. use13C marks carbon element in urea, also called carbon [ C ]13C-Urea [ sic ]13CO(NH2)2Or carbon [ C ]13C-Urea, carried thereby13C is12An isotope of C. If helicobacter pylori (Hp) is present in the stomach of a patient, the urease produced will break down the urea into13CO2Checking in the expired air of the patient with a matching instrument13C, the infection of helicobacter pylori (Hp) can be diagnosed. Comprises13C-labelled carbon [13C-urea large-scale preparation technology and process are always industrial difficulties. The invention is based on Franz r.a. and applegathf13C-Urea preparation, the basic principle is described in organic chemistry (1961), volume 26, page 2604-2605, and the chemical equation of the reaction is as follows:
13CO+S+2NH3→H2N13CONH2+H2S
however, the prior art can not realize the large-scale operation on the basis of the prior artScale production of carbon [13C-Urea. The main innovation point of the invention is that the raw material gas is filled in the pressure-resistant reaction kettle by using a cooling technology, so that the reaction system is13CO and NH3The S is a solid state, and the content of substances in unit reaction volume is greatly improved; the temperature is increased to ensure that the conditions in the reaction kettle reach the required conditions for urea synthesis, and carbon (C) is realized13C-Large-Scale preparation of Urea.
FIG. 1 shows carbon [ according to the invention ]13C-Process of the preferred embodiment of Urea Synthesis control method, as shown in FIG. 1, the carbon [ C ] of this embodiment13C-urea synthesis control method, comprising the following steps:
s100, filling raw materials: weighing methanol and sulfur, putting into a reaction kettle, cooling the reaction kettle by using liquid nitrogen, and sequentially communicating13CO and NH3To finish13CO and NH3Filling the liquefied mixture into a reaction kettle; methanol is used as a reaction medium in the urea synthesis process; because there is pressure differential between reation kettle and the raw materials gas cylinder, the feed gas flows into reation kettle from the raw materials gas cylinder, is liquid at the inside cooling of reation kettle, therefore the feed gas flows into reation kettle and can not lead to reation kettle internal pressure to rise, as long as the output pressure of raw materials gas cylinder remains stable promptly, and the pressure differential between reation kettle and the raw materials gas cylinder can continuously exist, and the feed gas can continuously fill and get into reation kettle.
S200, urea synthesis reaction: and (3) sealing the reaction kettle, controlling the temperature to 80-120 ℃, detecting the pressure value in the reaction kettle until the pressure in the reaction kettle is reduced to be constant, and finishing the reaction.
In the step S100, because there is pressure difference between the reaction kettle and the raw material gas cylinder, the raw material gas flows into the reaction kettle from the raw material gas cylinder, and is cooled to be liquid inside the reaction kettle, so that the raw material gas flows into the reaction kettle without causing pressure rise in the reaction kettle, that is, as long as the output pressure of the raw material gas cylinder remains stable, the pressure difference between the reaction kettle and the raw material gas cylinder can continuously exist, and the raw material gas can continuously be filled into the reaction kettle. The amount of material added can be adjusted to the yield per batch, for example 2.0mol carbon per batch13C-Urea Synthesis according to the weights of the materials listed in Table 1Sulfur and methanol were manually weighed and charged into a reaction kettle. The autoclave was placed in a liquid nitrogen bath and, when reduced to the appropriate temperature, ammonia gas and the corresponding weights as listed in Table 1 were added13CO was added to the reactor. Due to ammonia gas and ammonia gas in the reaction kettle13The CO is liquid and requires that the reactor be able to withstand a certain pressure, for example 3000 psig.
Carbon [ can be produced using the compounds of Table 1 below and their corresponding purities13C ] crude urea, 2.0mol per reactor. It is noted that except for13CO, all other materials are fed in excess to ensure consumption13The reaction of CO can occur at 100%.
TABLE 1
In the process of filling the raw materials, the temperature range in the reaction kettle is-160 to-200 ℃, and the pressure is-14 to-10 psig;13the filling stage of the CO is carried out,13the CO output pressure is 30-100 psig; NH (NH)3Filling stage, NH3The output pressure is 50-200 psig.
In step S200, the pressure in the reaction kettle is gradually reduced along with the urea synthesis reaction; the pressure in the reaction kettle is less than 1500psig when the urea synthesis reaction is just started, and the pressure in the reaction kettle is 100-200 psig when the urea synthesis reaction is completed. After the completion of the raw material filling, the reaction kettle was returned to room temperature. They were then placed on a rocking system and a heating mantle automatically controlled the reaction temperature to 100 ℃. + -. 20 ℃. The pressure varies within a certain range based on the amount of ammonia in the liquid phase in the reaction vessel, and at 2.0mol of the batch, the pressure in the reaction vessel at the very beginning of the reaction is 1000 to 1500 psig. The rocking system slowly rocked the autoclave to reduce the time required for complete reaction. The temperature and pressure were closely monitored and if the reactor pressure remained stable for 2h (no pressure change) this indicated the end of the reaction. The reaction time per 2.0mol of reactor batch is generally not more than 6 h.
In another preferred embodiment of the present invention, step S100 further includes the following steps:
s010, purging a reaction kettle: helium was used to evacuate the air from the autoclave. The helium output pressure is greater than the pressure in the reaction kettle; the output pressure of helium is 10-15 psig, and the pressure in the reaction kettle is 0-5 psig.
In another preferred embodiment of the present invention, the step S200 further includes the following steps:
s300, waste gas removal: and (3) exhausting residual waste gas in the reaction kettle after the urea synthesis reaction is finished by using nitrogen. The output pressure of the nitrogen is greater than the pressure in the reaction kettle; the output pressure of the nitrogen source is 10-15 psig, and the pressure in the reaction kettle is 0-5 psig. After the reaction was complete, the reactor was moved to a purge manifold to remove excess ammonia (NH)3) And hydrogen sulfide (H) as a by-product2S). The reactor was purged with nitrogen and the contents transferred to a scrubber to neutralize the by-products. And after the purging of the reactor is finished, placing the reaction kettle in a floor fume hood for collection.
In another preferred embodiment of the invention, carbon [ C ]13C, the urea synthesis process also comprises a gas leakage monitoring step: the urea synthesis process is carried out in an operation chamber, the operation chamber is kept at negative pressure by using an air draft device, and the air draft device is communicated with an air draft pipeline; an ammonia gas sensing probe, a carbon monoxide sensing probe and a hydrogen sulfide sensing probe are respectively arranged in the operation room and the air exhaust pipeline, when the content of ammonia gas and/or carbon monoxide and/or hydrogen sulfide exceeds a preset value, gas leakage possibly occurs, and13CO、NH3、H2s can be a health hazard to the operator, the system alarming and/or immediately closing the associated valve. And (4) related operators need to monitor the air leakage of the pipeline and maintain the pipeline, and then continue to operate the urea synthesis process.
In another preferred embodiment of the invention, the carbon [ C ] produced13C, purifying the urea to obtain a pure product with the purity of over 99 percent. The mother liquor was collected in a glass flask, then placed on a rotary evaporator to remove sulfur and dried. Through the treatment of the stepThe latter material is called "carbon13C-Urea crude product.
While the present invention has been described with reference to the embodiments shown in the drawings, the present invention is not limited to the embodiments, which are illustrative and not restrictive, and it will be apparent to those skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. A kind of13The C-urea synthesis control method is characterized by comprising the following steps:
s100, filling raw materials: weighing methanol and sulfur, putting into a reaction kettle, cooling the reaction kettle by using liquid nitrogen, and sequentially communicating13CO and NH3To finish13CO and NH3Filling the liquefied mixture into a reaction kettle; in the step S100, the temperature range in the reaction kettle is-160 to-200 ℃, and the pressure is-14 to-10 psig;13the filling stage of the CO is carried out,13the CO output pressure is 30-100 psig; NH (NH)3Filling stage, NH3The output pressure is 50-200 psig;
s200, urea synthesis reaction: and sealing the reaction kettle, controlling the temperature to be 80-120 ℃, and detecting the pressure value in the reaction kettle until the pressure in the reaction kettle is reduced to be constant, so that the reaction is finished.
2. The method of claim 113The C-urea synthesis control method is characterized by further comprising the following steps before the step S100:
s010, purging a reaction kettle: helium was used to evacuate the air from the autoclave.
3. The method of claim 213The C-urea synthesis control method is characterized in that in the step S010, helium output pressure is greater than pressure in the reaction kettle; the output pressure of helium is 5-15 psig, and the pressure in the reaction kettle is 0-5 psig.
4. The method of claim 113The C-urea synthesis control method is characterized in that in the step S200, the pressure in the reaction kettle is gradually reduced along with the urea synthesis reaction; the pressure in the reaction kettle is less than 1500psig when the urea synthesis reaction is just started, and the pressure in the reaction kettle is 100-200 psig when the urea synthesis reaction is completed.
5. The method of claim 113The C-urea synthesis control method is characterized by further comprising the following steps after the step S200:
s300, waste gas removal: and (3) exhausting residual waste gas in the reaction kettle after the urea synthesis reaction is finished by using nitrogen.
6. The method of claim 513The C-urea synthesis control method is characterized in that in the step S300, the output pressure of nitrogen is greater than the pressure in the reaction kettle; the output pressure of the nitrogen source is 10-15 psig, and the pressure in the reaction kettle is 0-5 psig.
7. The method of claim 113The C-urea synthesis control method is characterized by further comprising the following air leakage monitoring step: in the urea synthesis process, an air draft device is used for keeping the operating room at negative pressure; an ammonia gas sensing probe, a carbon monoxide sensing probe and a hydrogen sulfide sensing probe are respectively arranged in the operation room and the air exhaust pipeline, and when the content of ammonia gas and/or carbon monoxide and/or hydrogen sulfide exceeds a preset value, the system gives an alarm.
8. The method of claim 113The C-urea synthesis control method is characterized in that the reaction kettle can resist 3000psig pressure.
9. The method of claim 113A C-urea synthesis control method is characterized in that,13the synthesis efficiency of the C-urea is between 70 and 95 percent, and the produced C-urea13The purity of the C-urea is obtained by a purification processMore than 99% of pure product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610599129.8A CN107663162B (en) | 2016-07-27 | 2016-07-27 | A kind of13C-urea synthesis control method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610599129.8A CN107663162B (en) | 2016-07-27 | 2016-07-27 | A kind of13C-urea synthesis control method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107663162A CN107663162A (en) | 2018-02-06 |
| CN107663162B true CN107663162B (en) | 2020-06-30 |
Family
ID=61114947
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610599129.8A Active CN107663162B (en) | 2016-07-27 | 2016-07-27 | A kind of13C-urea synthesis control method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107663162B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108395385B (en) * | 2018-03-08 | 2020-11-13 | 江苏华益科技有限公司 | Isotope urea and its synthesis method |
| CN111205205B (en) * | 2020-01-19 | 2022-11-25 | 上海化工研究院有限公司 | Preparation method of O-18 labeled urea |
| CN115197100B (en) * | 2022-07-26 | 2024-08-06 | 深圳市中核海得威生物科技有限公司 | The method comprises the following steps of13Continuous flow synthesis method of C-urea |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2393141C1 (en) * | 2008-12-01 | 2010-06-27 | Общество с ограниченной ответственностью "Ростхим" (ООО "Ростхим") | 13c-urea synthesis method |
| CN105294510A (en) * | 2015-11-19 | 2016-02-03 | 上海化工研究院 | Stable isotope 13C or 15N-labeled biurea synthesis method |
-
2016
- 2016-07-27 CN CN201610599129.8A patent/CN107663162B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2393141C1 (en) * | 2008-12-01 | 2010-06-27 | Общество с ограниченной ответственностью "Ростхим" (ООО "Ростхим") | 13c-urea synthesis method |
| CN105294510A (en) * | 2015-11-19 | 2016-02-03 | 上海化工研究院 | Stable isotope 13C or 15N-labeled biurea synthesis method |
Non-Patent Citations (2)
| Title |
|---|
| "Syntheses with stable isotopes. Urea-13C, urea-12C, and urea-13C-15N2";Whaley, Thomas W.等;《Journal of Labelled Compounds》;19751231;第11卷(第2期);第169页 * |
| Carlos R. Sant Ana Filho等."SÍNTESE E CONTROLE DE QUALIDADE DA UREIA ENRIQUECIDA EM 13C PARA DIAGNÓSTICO DA Helicobacter pylori (HP)".《Quim. Nova》.2012,第36卷(第1期),第107-113页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107663162A (en) | 2018-02-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107663162B (en) | A kind of13C-urea synthesis control method | |
| EP2106385B1 (en) | Method for producing a hydrogen enriched fuel using microwave assisted methane plasma decomposition on catalyst | |
| CN108484924B (en) | Nickel coordination polymer for separating acetylene/ethylene mixed gas and preparation method thereof | |
| Kong et al. | In situ fabrication of high-permeance ZIF-8 tubular membranes in a continuous flow system | |
| Chen et al. | Structure, adsorption and magnetic properties of chiral metal–organic frameworks bearing linear trinuclear secondary building blocks | |
| CN104203824A (en) | Zeolite and method for producing same, and cracking catalyst for paraffin | |
| WO2024066073A1 (en) | Use of chlorine-free catalyst in preparation of diisopropylaminosilane | |
| CN108084105A (en) | Gadoteridol intermediate and its synthetic method and the method for preparing Gadoteridol using the Gadoteridol intermediate | |
| CN113804534B (en) | Offline pretreatment device and method for carbonate cluster isotope delta 47 | |
| CN108178770A (en) | A kind of method for synthesizing alpha-amido boron compound | |
| CN109180510B (en) | Preparation method of high-purity ferrous glutamate | |
| EP4324809A1 (en) | Continuous-flow synthesis method of 13c-urea | |
| CN109896978B (en) | 14Synthesis method of C-urea | |
| CN107663163B (en) | Is used for13Raw material gas filling method for C-urea synthesis | |
| CN110698686B (en) | Terbium coordination polymer for separating propyne/propylene mixed gas and preparation method thereof | |
| CN112500582B (en) | Multinuclear cobalt cluster metal organic framework material based on four-head pyrazole ligand, preparation and application | |
| CN103936079A (en) | High-stability material for producing synthetic gas and preparation method of material | |
| CN105771697A (en) | Coordination polymer membrane material modified by hydrophobic polymer coating as well as preparation method and application of coordination polymer membrane material | |
| CN110483505A (en) | 2- phenylimidazole [1,2-a] pyridine -3- nitrile replaced using DMF and ammonium iodide as cyanylation agent building | |
| CN215924817U (en) | Utilize device of 2-chlorine-5-chloromethyl pyridine waste gas synthesis ethylidene amino acid ethyl ester hydrochloride | |
| CN108440327B (en) | Method for preparing heptafluoroisobutyl amide from bis- (heptafluoroisopropyl) -ketone and ammonia | |
| CN114249627B (en) | Method for preparing E-1-chloro-3, 3, 3-trifluoropropene | |
| Cui et al. | Crystal Structure of a 1D Silver (I) Coordination Polymer Containing Flexible bis (benzimidazole) | |
| CN109896979B (en) | 14Production system of C-urea | |
| CN107661733B (en) | Is used for13Reaction kettle for synthesizing C-urea |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |