CN1289488C - Method and catalyst for preparing 2-cyanopyrazine by ammoxidation - Google Patents
Method and catalyst for preparing 2-cyanopyrazine by ammoxidation Download PDFInfo
- Publication number
- CN1289488C CN1289488C CN 03101166 CN03101166A CN1289488C CN 1289488 C CN1289488 C CN 1289488C CN 03101166 CN03101166 CN 03101166 CN 03101166 A CN03101166 A CN 03101166A CN 1289488 C CN1289488 C CN 1289488C
- Authority
- CN
- China
- Prior art keywords
- ammonia
- catalyzer
- catalyst
- methylpyrazine
- oxidation
- 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.)
- Expired - Fee Related
Links
- 239000003054 catalyst Substances 0.000 title claims abstract description 24
- PMSVVUSIPKHUMT-UHFFFAOYSA-N cyanopyrazine Chemical compound N#CC1=CN=CC=N1 PMSVVUSIPKHUMT-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 36
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 18
- 239000010936 titanium Substances 0.000 claims abstract description 15
- 230000003647 oxidation Effects 0.000 claims abstract description 13
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011651 chromium Substances 0.000 claims abstract description 10
- 239000010949 copper Substances 0.000 claims abstract description 8
- 239000011777 magnesium Substances 0.000 claims abstract description 8
- 239000011701 zinc Substances 0.000 claims abstract description 8
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 6
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052796 boron Inorganic materials 0.000 claims abstract description 6
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 6
- 229910052802 copper Inorganic materials 0.000 claims abstract description 6
- 230000000694 effects Effects 0.000 claims abstract description 6
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 6
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 6
- 239000011733 molybdenum Substances 0.000 claims abstract description 6
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 6
- 239000011574 phosphorus Substances 0.000 claims abstract description 6
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 6
- 239000011591 potassium Substances 0.000 claims abstract description 6
- 229910052718 tin Inorganic materials 0.000 claims abstract description 6
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 6
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000010941 cobalt Substances 0.000 claims abstract description 5
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 5
- 239000011135 tin Substances 0.000 claims abstract description 5
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims abstract description 4
- CAWHJQAVHZEVTJ-UHFFFAOYSA-N methylpyrazine Chemical compound CC1=CN=CC=N1 CAWHJQAVHZEVTJ-UHFFFAOYSA-N 0.000 claims description 28
- 238000006243 chemical reaction Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000000741 silica gel Substances 0.000 claims description 7
- 229910002027 silica gel Inorganic materials 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 4
- 239000004480 active ingredient Substances 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims 1
- 229910052720 vanadium Inorganic materials 0.000 abstract description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052719 titanium Inorganic materials 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 8
- 230000009466 transformation Effects 0.000 description 6
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 4
- 239000011572 manganese Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000005915 ammonolysis reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 125000004093 cyano group Chemical group *C#N 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- 229910013553 LiNO Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- NIPZZXUFJPQHNH-UHFFFAOYSA-N pyrazine-2-carboxylic acid Chemical compound OC(=O)C1=CN=CC=N1 NIPZZXUFJPQHNH-UHFFFAOYSA-N 0.000 description 1
- IPEHBUMCGVEMRF-UHFFFAOYSA-N pyrazinecarboxamide Chemical group NC(=O)C1=CN=CC=N1 IPEHBUMCGVEMRF-UHFFFAOYSA-N 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
Landscapes
- Catalysts (AREA)
Abstract
The invention discloses a method for preparing 2-cyanopyrazine by ammonia oxidation and a special catalyst, which is a multi-component catalyst taking vanadium and titanium as main catalysts and phosphorus, iron, nickel, cobalt, bismuth, manganese, chromium, molybdenum, copper, zinc, tin, boron, potassium, lithium, magnesium and the like as auxiliary catalysts: vaTibPcDdEeOx. The catalyst is used for preparing 2-cyanopyrazine by an ammoxidation method, and has the advantages of high activity, good selectivity, high product yield, high purity, simple process and the like.
Description
One, technical field
The present invention relates to method and special-purpose catalyst that a kind of oxidation proceses of ammonia prepares 2 cyano pyrazine, it belongs to technical field of organic chemistry, also belongs to organic fine chemical technical field.
Two, background technology
2 cyano pyrazine, molecular formula C
5H
3N
3, white or light yellow liquid under the normal temperature.Be applied to industries such as medicine, spices.
Because the 2-methylpyrazine makes 2 cyano pyrazine through oxidative ammonolysis under catalyst action is the method for preparing the best of cyano group compounds at present, its key is to find the catalyzer of high reactivity, highly selective.Ammonia oxidation is meant under catalyst action, labile methyl group in the organic molecule and cheap ammonia and oxygen (air) reaction, and a step is converted into the catalyzed reaction of cyano group.The preparation of employing oxidation proceses of ammonia, 2 cyano pyrazine have technology simple and direct, can carry out continuously, advantage such as throughput is strong, environmentally friendly and raw material is easy to get, other traditional synthesis that alternative route is long, energy consumption is high, environmental pollution is serious is produced the method for 2 cyano pyrazine.At present, using oxidation proceses of ammonia in the world prepares the 2 cyano pyrazine method and does not appear in the newspapers, domestic rarely seen TQ463 report adopts the CP-2 loaded catalyst to carry out the research that the direct ammonia oxidation of 2-methylpyrazine prepares 2 cyano pyrazine, and suitable temperature of reaction is 430 ℃, and reactant ratio is n (NH
3): n (O
2): n (H
2O)=1: (10~15): 2: 5, it was about 90% to reach reaction conversion ratio, and the 2 cyano pyrazine selectivity is about 80%.
Three, summary of the invention
The purpose of this invention is to provide method and special-purpose catalyst that a kind of ammonia oxidation prepares 2 cyano pyrazine, this catalyzer answers that cost is low, thermostability and physical strength are good, better selectivity of tool and activity can improve the transformation efficiency of 2-methylpyrazine and the productive rate of 2 cyano pyrazine.
For realizing that the present invention adopts following measure:
A kind of ammonia oxidation prepares the catalyzer of 2 cyano pyrazine, and it is to be Primary Catalysts with vanadium, titanium, and phosphorus, iron, nickel, cobalt, bismuth, manganese, chromium, molybdenum, copper, zinc, tin, boron, potassium, lithium, magnesium etc. are the multicomponent catalyst of helping agent, and it consists of: V
aTi
bP
cD
dE
eO
x/ SiO
2, wherein P is that phosphorus, D are iron, nickel, cobalt, bismuth, manganese, chromium, molybdenum, E is copper, zinc, tin, boron, potassium, lithium or magnesium; A=1; B=0.3~2.5; C=0.5~1.7; D=0~1.2; E=0~0.9; X then decides according to the content of above each element.Active ingredient element wt content is 5~30%, and preferably scope is 8~20%.Carrier is a microsphere silica gel, and the microsphere diameter scope is 125~450m.
Preparation of catalysts adopts pickling process: oxide compound, salt or the alkali of each element of the effective constituent of catalyzer dissolved respectively, mixes, fully flood the back stirring with carrier silica gel again, and still aging, under suitable temperature, activate certain hour then.Generally between 713~903K, preferably temperature range is 763~843K to activation temperature.Soak time was generally 4~12 hours, and the optimum activating time scope is 5~11 hours.
Preparation is during catalyzer, and each component can be with oxide compound, salt or the alkali etc. of this element.For example vanadium can be used NH
4VO
3, titanium can be used TiCl
4, Ti
2(C
2O
4)
3Deng, phosphorus can be used H
3PO
4, (NH
4)
3PO
4, (NH
4)
2HPO
4, (NH
4) H
2PO
4Or P
2O
5Deng, manganese can be used MnO
2, MnCl
2, Mn (NO
3)
2Deng, chromium can be used CrCl
3, Cr (NO
3)
39H
2O, Cr
2O
3, CrO
3Or (NH
4)
2Cr
2O
7Deng, molybdenum can be used MoO
3, (NH
4)
6Mo
7O
24Deng, iron can be used FeCl
3, Fe
2O
3, Fe
3O
4, Fe (NO
3)
39H
2O, Fe (OAc)
2, Fe (C
2O
4) 2H
2O or Fe
2(C
2O
4) 6H
2O etc., copper can be used CuCl
2Or Cu (NO
3)
2Deng, zinc can be used ZnO, ZnCl
2, Zn (NO
3)
2Or Zn (OAc)
22H
2O etc., tin can be used SnCl
2Or SnCl
4Deng, boron can be used H
3BO
3, potassium can be used KOH, KCl, KNO
3, K
2CO
3Or K
2C
2O
4Deng, lithium can be used Li
2O, LiCl, LiNO
3Or Li
2CO
3Deng, magnesium can be used MgO, MgCl
2Or Mg (NO
3)
26H
2O etc.
The optimum process condition scope of the open catalyzer oxidative ammonolysis of the present invention is as follows: temperature of reaction 633~713K, the mol ratio of air and 2-methylpyrazine is 8~60, the mol ratio of ammonia and 2-methylpyrazine is 2~12, catalyst loading 30~100g (kgcath).Be that the transformation efficiency of 2-methylpyrazine can be higher than 97.0% on the steel pipe fixed-bed reactor of 30mm and under the stable reaction conditions at internal diameter, the molar yield of 2 cyano pyrazine can be up to 88.5%, and product purity is higher than 97.0%.
Adopting with vanadium, titanium among the present invention is Primary Catalysts, phosphorus, iron, nickel, cobalt, bismuth, chromium, molybdenum, copper, zinc, tin, boron, potassium, lithium, magnesium etc. are five component catalysts of promotor, can make the 2-methylpyrazine make 2 cyano pyrazine, the method that traditional synthesis that can alternative route is long, energy consumption is high, environmental pollution is serious is produced 2 cyano pyrazine through oxidative ammonolysis one step.Simultaneously, this catalyzer uses silica gel to make carrier, face carrier silica gel can provide the effective ratio area and the pore structure of catalyzed reaction, the thermostability and the physical strength of catalyzer have been improved greatly, reduced the usage quantity of catalyst activity component, the Preparation of catalysts cost is reduced, on fixed bed and fluidized-bed reactor, all can use.
Four, embodiment
Below in conjunction with embodiment, the technology of the present invention is described in further detail.
Embodiment 1
With 4.431 gram H
2C
2O
42H
2O is dissolved under 85 ℃ in the 30mL distilled water, adds the TiCl of 1.11 grams, 85% strong phosphoric acid, 3.211 gram vanadium and 11.60mL 0.139mol/L then respectively
4Solution after the uniform solution to be formed, is poured solution into 30 gram silica gel (among the Φ 125~425um).Stir, after the drying, in muffle furnace, progressively be warmed up to 550 ℃, calcination 10 hours with 70 ℃ heat-up rate per hour.Standby behind the naturally cooling.Consisting of of catalyzer: V
1Ti
1.3P
0.5/ SiO
2, activity of such catalysts composition weight content is 10%.
At internal diameter is the above-mentioned solid catalyst of filling 15g in the steel pipe fixed-bed reactor of 30mm, and the mole proportioning of reaction raw materials is the 2-methylpyrazine: ammonia: air=1: 6: 15, temperature of reaction are 683K, and the load of catalyzer is 50g/ (kgcath).After reacting for 15 seconds, the transformation efficiency 89.7% of 2-methylpyrazine, the molar yield of 2 cyano pyrazine is 81.2%, and the selectivity of 2 cyano pyrazine is 81.8%, and product purity is 97.5%.
Embodiment 2~4: catalyzer is formed different, and processing condition are with embodiment 1, result such as following table:
Embodiment | Catalyzer | Transformation efficiency % | Productive rate % | Selectivity % |
2 | V 1Ti 0.4P 1.4Bi 0.1/SiO 2 | 97.7 | 83.4 | 83.5 |
3 | V 1Ti 1.8P 0.4K 0.2/SiO 2 | 98.4 | 84.2 | 84.7 |
4 | V 1Ti 21P 0.8Cr 0.2/SiO 2 | 98.2 | 85.7 | 86.4 |
Embodiment 5
With 4.403 gram H
2C
2O
42H
2O is dissolved under 85 ℃ in the 30mL distilled water, sweeps then not add 4.4296 grams, 85% strong phosphoric acid, 3.132 gram vanadium, behind the dark blue solution to be formed, adds TiCl O.139mol/L
4Solution 2.65mL, 50%Mn (NO
3)
2Solution 2.2946mL and O.1202 restrain LiCl after the uniform solution to be formed, pours solution rapidly in the 30 gram silicon (Φ 125~425 μ m).Stir, placement is spent the night.In High Temperature Furnaces Heating Apparatus, progressively be warmed up to 550 ℃, calcination 1O hour.After treating naturally cooling, preserve stand-by.Consisting of of this catalyzer: V
1Ti
0.3P
1.6Mn
0.25Li
0.2/ SiO
2, activity of such catalysts composition weight content is 10%.
The 15g catalyzer is packed in the internal diameter 30mm steel pipe fixed-bed reactor, and material mixed gas passes through catalyst bed reaction.Consisting of of material mixed gas: 2-methylpyrazine: ammonia: air=1: 6: 20.Temperature of reaction is 683K, and the load of catalyzer is 50g/ (kgcath).After reacting for 15 seconds, 2-methylpyrazine transformation efficiency 97.1%, 2 cyano pyrazine productive rate 87.5%, selectivity 90.3%, product purity 97.7%.Major impurity in the product is pyrazinoic acid amide and the pyrazine-2-formic acid that the 2-methylpyrazine generates in ammonia oxidation.
Embodiment 6~7: catalyzer is formed different, and processing condition are with embodiment 5, result such as following table:
Embodiment | Catalyzer | Transformation efficiency % | Productive rate % | Selectivity % |
6 | V 1Ti 2.2P 0.7Fe 0.2Mg 0.1/SiO 2 | 98.3 | 86.9 | 87.5 |
7 | V 1Ti 0.9P 0.5Cu 0.1B 0.15/SiO 2 | 97.7 | 87.7 | 88.9 |
Claims (4)
1, a kind of oxidation proceses of ammonia prepares the catalyzer of 2 cyano pyrazine, and it is to be carrier with silica gel, it is characterized in that: this catalyst activity composition consists of: V
aTi
bP
cD
dE
eO
x, wherein P=phosphorus, D=iron, nickel, cobalt, bismuth, manganese, chromium, molybdenum, E=copper, zinc, tin, boron, potassium, lithium or magnesium; A=1; B=0.3~2.5; C=0.5~1.7; D=0~1.2; E=0~0.9; X then decides according to the content and the valence state of above each element.
2, catalyzer according to claim 1 is characterized in that: the content of its active ingredient element is: 5~30%.
3, catalyzer according to claim 1 and 2 is characterized in that: the content of its active ingredient element is 8~20%.
4, oxidation proceses of ammonia prepares the method for 2 cyano pyrazine, it is characterized in that: oxide compound, salt or the alkali of each element of the active principle of claim 1 are dissolved mixing respectively, with carrier silica gel dipping, fully stirring, still aging again, between 713~903K, activate 4~12 hours then; The processing condition of ammonia oxidation: temperature of reaction 633~713K, the mol ratio of air and 2-methylpyrazine is 8~60, ammonia and 2-methylpyrazine mol ratio are 2~12, catalyst loading 30~100g/ (kgcath).
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 03101166 CN1289488C (en) | 2003-01-15 | 2003-01-15 | Method and catalyst for preparing 2-cyanopyrazine by ammoxidation |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN 03101166 CN1289488C (en) | 2003-01-15 | 2003-01-15 | Method and catalyst for preparing 2-cyanopyrazine by ammoxidation |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1429820A CN1429820A (en) | 2003-07-16 |
CN1289488C true CN1289488C (en) | 2006-12-13 |
Family
ID=4789914
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN 03101166 Expired - Fee Related CN1289488C (en) | 2003-01-15 | 2003-01-15 | Method and catalyst for preparing 2-cyanopyrazine by ammoxidation |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN1289488C (en) |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100427473C (en) * | 2006-11-21 | 2008-10-22 | 浙江大学 | Synthesis method of key intermediate 2-cyanpyrazine of tuberculosis drug pyrazinamide |
WO2013138227A1 (en) * | 2012-03-13 | 2013-09-19 | Celanese International Corporation | Catalyst for producing acrylic acids and acrylates |
CN106111172B (en) * | 2016-06-22 | 2018-06-15 | 徐州恒鼎生物科技有限公司 | Catalyst for preparing 3-cyanopyridine by catalytic ammoxidation and preparation method thereof |
CN109482211A (en) * | 2017-09-09 | 2019-03-19 | 中国石油化工股份有限公司 | A kind of catalyst and preparation method thereof for synthesizing 2 cyano pyrazine |
CN111410636A (en) * | 2020-03-30 | 2020-07-14 | 苏州弘森药业股份有限公司 | Preparation process of pyrazinamide |
-
2003
- 2003-01-15 CN CN 03101166 patent/CN1289488C/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
CN1429820A (en) | 2003-07-16 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101433836A (en) | Catalyst for producing 3-cyano pyridine as well as preparation method and use thereof | |
CN1137779C (en) | Method for preparing 3,4-dichlorophenylnitrile by using ammonia oxidation process and its special-purpose catalyst | |
CN103896807A (en) | Preparation method of terephthalonitrile through ammonium oxidation | |
CN103041838A (en) | Catalyst for preparing 2, 6-dichlorobenzonitrile from 2, 6-dichlorotoluene by means of ammoxidation | |
CN109876837B (en) | Special catalyst for preparing o-chlorobenzonitrile by ammoxidation method, preparation method and application thereof | |
CN1289488C (en) | Method and catalyst for preparing 2-cyanopyrazine by ammoxidation | |
CN101992091B (en) | Unsaturated nitrile fluid catalyst prepared by ammoxidation and preparation method thereof | |
CN103418405B (en) | Replenishment catalyst for maintaining stabilization production of acrylonitrile device | |
CN101759596A (en) | Method for preparing 3,4-dichloro-cyanobenzene | |
CN102744090B (en) | Catalyst for ammoxidation preparation of 2,4-dichlorobenzonitrile | |
CN101147867B (en) | Fluidized bed catalyst for oxidation of propene ammonia | |
CN1092540C (en) | Fluidized bed catalyst for ammoxidation of propylene | |
CN101265213A (en) | Method for preparing alkylcyanophenyl | |
CN1137778C (en) | Method for preparing 2,4-dichlorophenylnitrile by using ammonia oxidation process and special-purpose catalyst | |
CN1125676C (en) | Catalyst for preparing phthaloylimide by ammonia oxidizing method and its preparing process and usage | |
CN101767014B (en) | Fluidized bed catalyst for producing acrylonitrile by propylene ammoxidation | |
CN100408172C (en) | Acrylonitrile fluid bed catalyst | |
CN103664696A (en) | Method for preparing cyanobenzene | |
CN102219710A (en) | Method for preparing cyanobenzene | |
CN100379493C (en) | Catalyst for synthesizing para-hydroxy-benzonitrile and its preparing method and use | |
CN1230459A (en) | Propylene ammonoxidating catalyst | |
CN101733117B (en) | High-stability fluid catalyst for producing acrylonitrile | |
CN101306372B (en) | Fluid bed catalyst for acrylonitrile production | |
CN101757940B (en) | Catalyst for preparing 3,4-dichlorobenzonitrile | |
CN112457214B (en) | Synthesis method of 4-nitrophthalonitrile |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
C19 | Lapse of patent right due to non-payment of the annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |