CN108774156A - A method of preparing 2,6- dichlorobenzonitriles - Google Patents
A method of preparing 2,6- dichlorobenzonitriles Download PDFInfo
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- CN108774156A CN108774156A CN201810967597.5A CN201810967597A CN108774156A CN 108774156 A CN108774156 A CN 108774156A CN 201810967597 A CN201810967597 A CN 201810967597A CN 108774156 A CN108774156 A CN 108774156A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/24—Preparation of carboxylic acid nitriles by ammoxidation of hydrocarbons or substituted hydrocarbons
- C07C253/28—Preparation of carboxylic acid nitriles by ammoxidation of hydrocarbons or substituted hydrocarbons containing six-membered aromatic rings, e.g. styrene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/188—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum, tungsten or polonium
- B01J27/19—Molybdenum
Abstract
The present invention relates to 2,6- dichlorobenzonitrile preparation fields, specifically disclose a kind of method preparing 2,6- dichlorobenzonitriles with 2,6- dichlorobenzyl chlorides for raw material.The present invention replaces expensive 2,6-DCT to prepare 2,6- dichlorobenzonitriles as reactant with cheap 2,6- dichlorobenzyl chlorides, greatly reduces production cost.
Description
Technical field
The present invention relates to 2,6- dichlorobenzonitrile preparation fields, are with 2,6- dichlorobenzyl chlorides more specifically to one kind
The method that raw material prepares 2,6- dichlorobenzonitriles.
Background technology
2,6- dichlorobenzonitriles also known as dichlobenil are a kind of important chemical intermediates, are widely used in herbicide, kill
The fields such as worm agent, medicine, dyestuff, high molecular material.
The method of synthesis 2,6- dichlorobenzonitriles is broadly divided into organic synthesis method and gas phase ammonia oxidation.Gas phase ammonoxidation method
Refer to that under the effect of the catalyst, reactant carries out ammoxidation reaction with the oxygen in ammonia, air and generates 2,6- dichloro-benzenes first
Nitrile.For gas phase ammonoxidation method compared with organic synthesis method, flow is simple, and low energy consumption, and pollution is small, and product yield and purity are high, are works
The more satisfactory method of industryization.
Up to the present, do not have both at home and abroad with the method that 2,6- dichlorobenzyl chlorides are raw material preparation 2,6- dichloro-benzenes first eyeballs.It is existing
All it is using 2,6- dichlorotoleune as raw material using the method that gas phase ammonoxidation method prepares 2,6- dichloro-benzenes first eyeballs.2,6- dichloromethanes
Benzene price is high, and it is expensive to produce 2,6- dichlorobenzonitriles as reactant with it, and 2,6- dichlorobenzyl chloride prices are less than 2,
It is of low cost to produce 2,6- dichlorobenzonitriles with it as reactant for the half of 6- dichlorotoleune.In addition, with 2,6- dichloromethanes
Benzene is raw material ammoxidation system 2, and the device of 6- dichlorobenzonitriles mostly uses fluid bed, and such as Chinese patent ZL97109006.8, this is
Since ammoxidation reaction thermal discharge itself is big, the thermal instability of reaction is high, can not solve to radiate and conduct heat to ask using fixed bed
Topic have to use complicated fluidized bed plant, and fluidisation state is of poor quality in fluidized-bed reactor, causes product yield inclined
It is low, and catalyst consumes for a long time, increases production cost.
It therefore, can be very in the method that 2,6- dichlorobenzyl chlorides are raw material preparation 2,6- dichlorobenzonitriles if inventing one kind
Industrial cost is reduced in big degree.If this method can also use fixed-bed reactor, further simplify work
Skill condition improves reaction yield, reduces production cost.
Invention content
In order to reduce industrial production cost, the invention discloses one kind with 2,6- dichlorobenzyl chlorides (No. CAS：2014-83-7)
The method for preparing 2,6- dichlorobenzonitriles for raw material.
The reaction equation of 2,6- dichlorobenzyl chloride ammoxidation 2,6- dichlorobenzonitriles is：
C7H5Cl3+2NH3+O2=C7H3Cl2N+NH4Cl+2H2O
Main side reaction is reacted for excessive oxidation, and reaction equation is：
2C7H5Cl3+6NH3+15O2=6NH4Cl+14CO2+2H2O
The invention discloses a kind of method preparing 2,6- dichlorobenzonitriles, step is：
After liquid ammonia vaporization, gas mixing is carried out with nitrogen, air；2,6- dichlorobenzyl chlorides are vaporized by steam simultaneously, and upper
It states mixed gas to preheat together, be reacted in reactor, 2,6- dichloro-benzenes is obtained by cooling, washing, centrifugal dehydration
Formonitrile HCN crude product.
Wherein, liquid ammonia gasification can the overpressure through liquid ammonia storage tank realized automatically into the methods of liquid ammonia evaporator；
Gas mixing can be realized by gas circulating compressor etc.；2,6- dichlorobenzyl chlorides can enter 2,6- dichlorobenzyl chlorides through metering pump
Evaporator makes 2,6- dichlorobenzyl chlorides vaporize by middle pressure steam；Product after reaction is gas, through portion's cooler (gas cooling
Device), quencher (chilled water (chw) spray thrower) cooling after, become solid suspended particle, enter back into water scrubber use chilling water spray side
Formula is washed, and further sprays remaining 2,6- dichlorobenzonitriles in gas, crude product is obtained by centrifuge dewatering.
By-product ammonium chloride yield is larger, and reactor outlet temperature needs to control at 300 DEG C or so, not so easy generator tube
Road blocks.Meanwhile carrying out washing using chilling water spray mode into water scrubber can also be such that ammonium chloride is dissolved in chilled water (chw), prevent
Only ammonium chloride blockage pipeline.
The purpose for adding nitrogen is that the oxygen content in whole system is made to reduce, and air is made to become oxygen denuded air.Suitably
Oxygen content is conducive to inhibit excessive oxidation reaction, improves the selectivity entirely reacted.Volume of the oxygen in oxygen denuded air contains
Amount is proper for 6~16%, and 9~12% more preferably, and 10% or so is best.
2,6- dichlorobenzyl chlorides in the above method, ammonia, oxygen denuded air molar ratio be 1:2~10:5~100, preferably 1:
3~6:10~50, most preferably 1:4~6:10~20.
Temperature general more difficult to control, heat supply and shifting of the industrial reactor that the present invention uses in ammoxidation strong exothermal reaction
Heat is that the sodium nitrite prepared by certain proportion and the fused salt formed after mixture of potassium nitrate thawing are adjusted, molten by adjusting
The temperature (abbreviation salt temperature) of salt adjusts the temperature of reactor, in practice it has proved that, when salt temperature is adjusted to 370~410 DEG C, preferably 380
At~400 DEG C, most preferably 390 DEG C, the generation that excessive oxidation can be inhibited to react improves the selectivity and yield of reaction.
The catalyst that the present invention selects can be existing, prepare different types of dichlorobenzonitrile applied to ammoxidation reaction
Technology in known catalyst, or a kind of catalyst (abbreviation DBN-1 types catalyst) disclosed by the invention.Its
In, can smoothly realize with 2,6- dichlorobenzyl chlorides to be that raw material prepares 2,6- dichloro-benzenes first using the catalyst disclosed in the prior art
The ammoxidation reaction of nitrile, but the yield of product and selectivity are relatively low.If the present invention is using DBN-1 type catalyst, not only product
Selectivity it is good, yield is also very high.
The preparation method of DBN-1 type catalyst is：
1) preparation of active presoma
Vfanadium compound, phosphorus compound, molybdenum compound are added in alcohols solvent, stirs and suspension is made, heat temperature raising,
Reaction temperature is 80 DEG C~160 DEG C, reaction pressure is reacted under being 0~-40kPa, reacts 4h~6h, cooled and filtered, filter
Cake drying at 100 DEG C~160 DEG C for 24 hours, roasts 4h~8h at 280 DEG C~400 DEG C；Wherein, alcohols solvent be n-hexyl alcohol,
It is one or more in isobutanol, benzyl alcohol.
2) prepared by semi-finished product
Active presoma obtained by step 1) is uniformly obtained into mixture with carrier, auxiliary agent, pore creating material, mix lubricant
Material, wherein the carrier is one or more in aluminium oxide, silica, titanium oxide；The auxiliary agent be cobalt compound and/
Or chromium compound；Also mixed material can be shaped and be dried.
3) it activates
Semi-finished product obtained by step 2) are lived under the oxygen denuded air atmosphere of oxygen content ranging from 3%~15%
Change, activation temperature is 400 DEG C~600 DEG C, and soak time is 2h~10h.
Fixed bed can be selected in the reactor of the present invention, can also select fluid bed, but in the other parameters for meeting the present invention
Under the conditions of, it can control temperature using fixed bed and move heat, no longer need to use complicated fluid bed, meanwhile, using solid
Fixed bed can also avoid in fluidized-bed reactor fluidize state it is of poor quality, product yield is relatively low, and catalyst consumes for a long time, production cost
High defect.
Further, in order to reduce production cost, CO in whole system is prevented2Too high levels, the gas after present invention washing
Body is after gas scrubbing cools down, and 75%, which enters gas-liquid separator, recycles to reduce production cost, and 25% is pumped into using exhaust fan
It is vented after incinerator burning.Gas after recycling is recycled together with supplement air by recycle compressor.It was verified that
The gas ratio of recycling and emptying is 1：When 3, the gas of the oxygen, emptying that have reacted and the air of supplement can reach flat
Weighing apparatus.Certainly, if having changed other production equipments to realize that the present invention, recycling and the gas ratio being vented may occur certain
Variation.
The 2,6- dichlorobenzyl chlorides of low cost can be made to pass through gas phase ammonoxidation method using the present invention and be converted into 2,6- dichloro-benzenes
Formonitrile HCN reduces production cost；Such as according to homemade DBN-1 types catalyst, the high income of 2,6- dichlorobenzonitriles, selectivity
It is good；Fixed bed also can be used, it is simple for process, avoid in fluidized-bed reactor fluidize state it is of poor quality, product yield is relatively low, catalyst
Long-term consumption, the high problem of production cost；If further gas recovery then can be recycled, further reduce the cost, very
It is suitble to the needs of large-scale industrial production.
Description of the drawings
Fig. 1 is the equipment and flow diagram that realization this method can use.
Specific implementation mode
The present invention is furtherd elucidate below by embodiment.
The preparation of DBN-1 type catalyst：
Embodiment 1：
In the reaction kettle with stirring, heating and condensation reflux unit, it is added with stirring 5000g n-hexyl alcohols and 1000g
Benzyl alcohol, then sequentially adds vanadic anhydride 630g, phosphatase 11 96g, ammonium heptamolybdate 106g, calcium carbonate 60g, and control temperature exists
90 DEG C~100 DEG C, reacted under -30kPa~-40kPa, the organic solvent of evaporation is back to instead after water condenser condenses
It answers in kettle, stops reaction after reacting 6h.Obtained slurry is separated by solid-liquid separation to obtain filter cake, filter cake is at 120 DEG C~140 DEG C
Then dry 18h roasts 8h at 300 DEG C~320 DEG C and obtains active presoma.
Active presoma is added in kneader, aluminium oxide 1524g, cobalt nitrate 87g, sesbania powder 100g, carboxylic is then added
Methylcellulose 50g is uniformly mixed, and suitable water then is added under continuous mediate, until material is suitable for extrusion.It mediates
Good material is transferred to the item that 5mm is squeezed into banded extruder, the ball of diameter 5mm is then cut into pelleter, spherical particle is at 110 DEG C
~120 DEG C of dryings for 24 hours, 8h are roasted at 480 DEG C~500 DEG C under the atmosphere of oxygen content 9%~11%.
Embodiment 2：
In the reaction kettle with stirring, heating and condensation reflux unit, it is added with stirring 5500g n-hexyl alcohols and 1100g
Then benzyl alcohol sequentially adds ammonium metavanadate 778g, phosphatase 11 38g, ammonium tetramolybdate 115g, calcium oxide 50g, control temperature is 120
DEG C~130 DEG C, reacted under -10kPa~-20kPa, the organic solvent of evaporation is back to reaction after water condenser condenses
In kettle, stop reaction after reacting 4h.Obtained slurry is separated by solid-liquid separation to obtain filter cake, filter cake is done at 120 DEG C~140 DEG C
Then dry 18h roasts 6h at 320 DEG C~340 DEG C and obtains active presoma.
Active presoma is added in kneader, aluminium oxide 1524g, chromic nitrate 527g, cobalt nitrate 58g, field is then added
Cyanines powder 100g, carboxymethyl cellulose 50g are uniformly mixed, and suitable water then is added under continuous mediate, until material is suitable for crowded
Until item.Kneaded material is transferred to the item that 6mm is squeezed into banded extruder, and the ball of diameter 6mm is then cut into pelleter, spherical
Particle 110 DEG C~120 DEG C dryings for 24 hours, roast 8h under the atmosphere of oxygen content 8%~9% at 500 DEG C~520 DEG C.
Embodiment of the method：
The reactor that following embodiments use is by taking fixed bed reactors as an example, and isometric reaction tube is the length of
4000mm, reactor caliber are 25mm, and it is 3500mm that catalyst, which uses DBN-1 type catalyst, filling height,.
Using 1000 tons of commercial plants are produced per year, the oxygen volume content in whole system is first made using nitrogen for following embodiments
It is reduced to 10%, the air circulation of whole system is made by gas circulating compressor, liquefied ammonia, which enters after evaporator vaporizes to enter, to follow
Ring gas line and nitrogen, air carry out gas mixing, while 2,6- dichlorobenzyl chloride enter makes 2,6- dichlorobenzyl chlorides in evaporator
Vaporization, then mixed with mixed gas, it is preheated together into preheating mixer after mixing, reactor, reaction is entered after preheating
Gas afterwards is cooled to 300 DEG C by air cooling, then so that product in quencher is reduced to 80~90 DEG C through circulating water spray, product
With solid suspended particle as chilled water (chw) enters water scrubber, again being remained in gas phase by way of chilling water spray inside water scrubber
Remaining a small amount of product sprays, and the solid for washing tower bottom goes centrifugal device dehydration packaging in a manner of interim acquisition.Washing
Gas phase removes other level-one gas scrubbing tower in tower, and temperature is reduced within 40 DEG C, and 75% gas enters gas-liquid separator
To reduce production cost, 25% gas, which is pumped into using exhaust fan after incinerator burns, to be vented for recycling.Gas after recycling with
Supplement air is recycled by recycle compressor together.
Embodiment 3：
The molar ratio of three kinds of raw material steams is：2,6- dichlorobenzyl chlorides：Ammonia：Air=1：3：10, by fixed bed inner salt temperature
390 DEG C, pressure 40KPa are adjusted to, catalyst is added, is reacted 12 hours.The conversion ratio 99.5% of product is selectively
67.2%, yield 66.9%.
Embodiment 4:
The molar ratio of three kinds of raw material steams is：2,6- dichlorobenzyl chlorides：Ammonia：Air=1：3：15, by fixed bed inner salt temperature
390 DEG C, pressure 40KPa are adjusted to, catalyst is added, is reacted 12 hours.The conversion ratio 99.5% of product is selectively
77.0%, yield 76.6%.
Embodiment 5:
The molar ratio of three kinds of raw material steams is：2,6- dichlorobenzyl chlorides：Ammonia：Air=1：4：20, by fixed bed inner salt temperature
390 DEG C, pressure 40KPa are adjusted to, catalyst is added, is reacted 12 hours.The conversion ratio 99.5% of product is selectively
79.7%, yield 79.3%.
Embodiment 6:
The molar ratio of three kinds of raw material steams is：2,6- dichlorobenzyl chlorides：Ammonia：Air=1：4：15, by fixed bed inner salt temperature
390 DEG C, pressure 40KPa are adjusted to, catalyst is added, is reacted 12 hours.The conversion ratio 99.5% of product is selectively
79.5%, yield 79.1%.
Embodiment 7:
The molar ratio of three kinds of raw material steams is：2,6- dichlorobenzyl chlorides：Ammonia：Air=1：5：20, by fixed bed inner salt temperature
390 DEG C, pressure 40KPa are adjusted to, catalyst is added, is reacted 12 hours.The conversion ratio 99.5% of product is selectively
83.9%, yield 83.5%.
Embodiment 8:
The molar ratio of three kinds of raw material steams is：2,6- dichlorobenzyl chlorides：Ammonia：Air=1：6：20, by fixed bed inner salt temperature
390 DEG C, pressure 40KPa are adjusted to, catalyst is added, is reacted 12 hours.The conversion ratio 99.5% of product is selectively
75.4%, yield 75.0%.
Embodiment 9:
The molar ratio of three kinds of raw material steams is：2,6- dichlorobenzyl chlorides：Ammonia：Air=1：6：15, by fixed bed inner salt temperature
390 DEG C, pressure 40KPa are adjusted to, catalyst is added, is reacted 12 hours.The conversion ratio 99.5% of product is selectively
79.8%, yield 79.4%.
Embodiment 10:
The molar ratio of three kinds of raw material steams is：2,6- dichlorobenzyl chlorides：Ammonia：Air=1：5：15, by fixed bed inner salt temperature
390 DEG C, pressure 40KPa are adjusted to, catalyst is added, is reacted 12 hours.The conversion ratio 99.5% of product is selectively
83.5%, yield 83%.
Embodiment 11:
The molar ratio of three kinds of raw material steams is：2,6- dichlorobenzyl chlorides：Ammonia：Air=1：5：15, by fixed bed inner salt temperature
380 DEG C, pressure 40KPa are adjusted to, catalyst is added, is reacted 12 hours.The conversion ratio 98.5% of product is selectively
80.8%, yield 79.6%.
Embodiment 12:
The molar ratio of three kinds of raw material steams is：2,6- dichlorobenzyl chlorides：Ammonia：Air=1：5：15, by fixed bed inner salt temperature
388 DEG C, pressure 40KPa are adjusted to, catalyst is added, is reacted 12 hours.The conversion ratio 99.5% of product is selectively
82.7%, yield 82.3%.
Embodiment 13:
The molar ratio of three kinds of raw material steams is：2,6- dichlorobenzyl chlorides：Ammonia：Air=1：5：15, by fixed bed inner salt temperature
395 DEG C, pressure 40KPa are adjusted to, catalyst is added, is reacted 12 hours.The conversion ratio 99.8% of product is selectively
82.6%, yield 82.4%.
Embodiment 14:
The molar ratio of three kinds of raw material steams is：2,6- dichlorobenzyl chlorides：Ammonia：Air=1：5：15, by fixed bed inner salt temperature
400 DEG C, pressure 40KPa are adjusted to, catalyst is added, is reacted 12 hours.The conversion ratio 100% of product is selectively
78.2%, yield 78.2%.
The present invention is not limited to the above embodiment the specific technical solution, all technical sides formed using equivalent replacement
Case is the range that the present invention is protected.
Claims (10)
1. a kind of method preparing 2,6- dichlorobenzonitriles, step are：After liquid ammonia vaporization, carries out gas with nitrogen, air and mix
It closes；2,6- dichlorobenzyl chlorides are vaporized by steam simultaneously, are preheated together with above-mentioned mixed gas, are reacted in reactor,
Salt temperature be 370~410 DEG C, 2,6- dichlorobenzyl chlorides, ammonia, oxygen denuded air molar ratio be 1:2~10:5~100, wherein oxygen
Volume content in oxygen denuded air is 6~16%；Catalyst is the catalyst that dichlorobenzonitrile is prepared using ammonia oxidation, warp
Cooling, washing, centrifugal dehydration are crossed, 2,6- dichlorobenzonitrile crude products are obtained.
2. the method according to claim 1 for preparing 2,6- dichlorobenzonitriles, it is characterised in that 2,6- dichlorobenzyl chlorides:Ammonia
Gas:The molar ratio of oxygen denuded air is 1:3~6:10~50.
3. the method according to claim 1 for preparing 2,6- dichlorobenzonitriles, it is characterised in that oxygen is in oxygen denuded air
Volume content 9~12%.
4. the method according to claim 1 for preparing 2,6- dichlorobenzonitriles, it is characterised in that salt temperature is 380 DEG C~400
℃。
5. the method according to claim 1 for preparing 2,6- dichlorobenzonitriles, it is characterised in that catalyst uses the present invention
A kind of disclosed catalyst, the preparation method of the catalyst are：
1) preparation of active presoma
Vfanadium compound, phosphorus compound, molybdenum compound are added in alcohols solvent, suspension is made in stirring, and heat temperature raising is reacting
Temperature is 80 DEG C~160 DEG C, reaction pressure is reacted under being 0~-40kPa, react 4h~6h, cooled and filtered, filter cake in
Drying for 24 hours, roasts 4h~8h at 280 DEG C~400 DEG C at 100 DEG C~160 DEG C；Wherein, alcohols solvent is n-hexyl alcohol, isobutyl
It is one or more in alcohol, benzyl alcohol；
2) prepared by semi-finished product
Active presoma obtained by step 1) is uniformly obtained into mixed material with carrier, auxiliary agent, pore creating material, mix lubricant, it will
Mixed material is molded and dries, wherein the carrier is one or more in aluminium oxide, silica, titanium oxide；Described
Auxiliary agent is cobalt compound and/or chromium compound；
3) it activates
Semi-finished product obtained by step 2) are activated under the oxygen denuded air atmosphere of oxygen content ranging from 3%~15%, it is living
It is 400 DEG C~600 DEG C to change temperature, and soak time is 2h~10h.
6. the method according to claim 1 for preparing 2,6- dichlorobenzonitriles, it is characterised in that reactor is that fixed bed is anti-
Answer device or fluidized-bed reactor.
7. the method according to claim 1 for preparing 2,6- dichlorobenzonitriles, it is characterised in that the gas after washing passes through
After wash cooling, a part is recycled into gas-liquid separator, after another part is pumped into incinerator burning using exhaust fan
Emptying.
8. the method according to claim 7 for preparing 2,6- dichlorobenzonitriles, it is characterised in that the gas after washing passes through
After wash cooling, 75% is recycled into gas-liquid separator, 25% be pumped into incinerator burning using exhaust fan after be vented.
9. a kind of method preparing 2,6- dichlorobenzonitriles, step are：Being passed through nitrogen reduces oxygen content, passes through gas circulation pressure
Contracting machine makes the gas circulation of whole system, liquefied ammonia are vaporized automatically into liquid ammonia evaporator using the overpressure of liquid ammonia storage tank
Enter recycle gas line afterwards and carry out gas mixing with nitrogen, air, while 2,6- dichlorobenzyl chloride enter evaporator through metering pump
In so that 2,6- dichlorobenzyl chlorides is vaporized, then mixed with above-mentioned mixed gas, preheated together into preheating mixer, preheating is laggard
Enter reactor to be reacted, salt temperature be 370~410 DEG C, 2,6- dichlorobenzyl chlorides, ammonia, oxygen denuded air molar ratio be 1:2~
10:5~100, wherein volume content of the oxygen in oxygen denuded air is 6~16%；Catalyst is to prepare two using ammonia oxidation
The catalyst of chlorobenzonitrile, the gas after reaction is cooled to 300 DEG C by portion's cooler, then makes in quencher through circulating water spray
Product is reduced to 80~90 DEG C, and product, as chilled water (chw) enters water scrubber, passes through chilling with solid suspended particle inside water scrubber
The mode of water spray is washed, and the solid for washing tower bottom goes centrifugal device to be dehydrated in a manner of interim acquisition；In water scrubber
Gas phase enter gas scrubbing tower, and gas temperature is reduced within 40 DEG C, 75% gas enters gas-liquid separator recycling,
25% gas is vented after being pumped into incinerator burning using exhaust fan；The gas of recycling is pressed together with supplement air by recycling
Contracting machine recycles.
10. the method according to claim 9 for preparing 2,6- dichlorobenzonitriles, it is characterised in that catalyst uses the present invention
A kind of disclosed catalyst, the preparation method of the catalyst are：
1) preparation of active presoma
Vfanadium compound, phosphorus compound, molybdenum compound are added in alcohols solvent, suspension is made in stirring, and heat temperature raising is reacting
Temperature is 80 DEG C~160 DEG C, reaction pressure is reacted under being 0~-40kPa, react 4h~6h, cooled and filtered, filter cake in
Drying for 24 hours, roasts 4h~8h at 280 DEG C~400 DEG C at 100 DEG C~160 DEG C；Wherein, alcohols solvent is n-hexyl alcohol, isobutyl
It is one or more in alcohol, benzyl alcohol；
2) prepared by semi-finished product
Active presoma obtained by step 1) is uniformly obtained into mixed material with carrier, auxiliary agent, pore creating material, mix lubricant, it will
Mixed material is molded and dries, wherein the carrier is one or more in aluminium oxide, silica, titanium oxide；Described
Auxiliary agent is cobalt compound and/or chromium compound；
3) it activates
Semi-finished product obtained by step 2) are activated under the oxygen denuded air atmosphere of oxygen content ranging from 3%~15%, it is living
It is 400 DEG C~600 DEG C to change temperature, and soak time is 2h~10h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109776356A (en) * | 2019-02-22 | 2019-05-21 | 江苏新河农用化工有限公司 | It is a kind of for synthesizing the trapping system and technique of 2,6- dichlorobenzonitrile |
| CN112047858A (en) * | 2020-09-03 | 2020-12-08 | 常州新日催化剂有限公司 | Trapping device and process for producing 2, 6-dichlorobenzonitrile |
| CN116854611A (en) * | 2023-07-06 | 2023-10-10 | 湖北纽苏莱新材料有限公司 | Method for preparing 2, 6-dichlorobenzonitrile by gas phase ammoxidation method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109776356A (en) * | 2019-02-22 | 2019-05-21 | 江苏新河农用化工有限公司 | It is a kind of for synthesizing the trapping system and technique of 2,6- dichlorobenzonitrile |
| CN109776356B (en) * | 2019-02-22 | 2022-03-25 | 江苏新河农用化工有限公司 | Trapping system and process for synthesizing 2, 6-dichlorobenzonitrile |
| CN112047858A (en) * | 2020-09-03 | 2020-12-08 | 常州新日催化剂有限公司 | Trapping device and process for producing 2, 6-dichlorobenzonitrile |
| CN112047858B (en) * | 2020-09-03 | 2021-03-26 | 常州新日催化剂股份有限公司 | Trapping device and process for producing 2, 6-dichlorobenzonitrile |
| CN116854611A (en) * | 2023-07-06 | 2023-10-10 | 湖北纽苏莱新材料有限公司 | Method for preparing 2, 6-dichlorobenzonitrile by gas phase ammoxidation method |
| CN116854611B (en) * | 2023-07-06 | 2024-04-23 | 湖北纽苏莱新材料有限公司 | Method for preparing 2, 6-dichlorobenzonitrile by gas phase ammoxidation method |
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