CN102432503A - Production method of pentachlorobenzonitrile - Google Patents
Production method of pentachlorobenzonitrile Download PDFInfo
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- CN102432503A CN102432503A CN2010102956914A CN201010295691A CN102432503A CN 102432503 A CN102432503 A CN 102432503A CN 2010102956914 A CN2010102956914 A CN 2010102956914A CN 201010295691 A CN201010295691 A CN 201010295691A CN 102432503 A CN102432503 A CN 102432503A
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- toluene
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- 238000004519 manufacturing process Methods 0.000 title abstract description 12
- INICGXSKJYKEIV-UHFFFAOYSA-N 2,3,4,5,6-pentachlorobenzonitrile Chemical compound ClC1=C(Cl)C(Cl)=C(C#N)C(Cl)=C1Cl INICGXSKJYKEIV-UHFFFAOYSA-N 0.000 title abstract 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 120
- 239000007789 gas Substances 0.000 claims abstract description 68
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 48
- JFDZBHWFFUWGJE-UHFFFAOYSA-N benzonitrile Chemical compound N#CC1=CC=CC=C1 JFDZBHWFFUWGJE-UHFFFAOYSA-N 0.000 claims abstract description 45
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 40
- 239000000460 chlorine Substances 0.000 claims abstract description 39
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 38
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 24
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000001301 oxygen Substances 0.000 claims abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 4
- 239000003570 air Substances 0.000 claims abstract description 3
- 239000006200 vaporizer Substances 0.000 claims description 32
- -1 pentachlorobenzene formonitrile Chemical compound 0.000 claims description 22
- 239000003610 charcoal Substances 0.000 claims description 16
- 238000009833 condensation Methods 0.000 claims description 16
- 230000005494 condensation Effects 0.000 claims description 16
- 230000000694 effects Effects 0.000 claims description 16
- 238000009834 vaporization Methods 0.000 claims description 16
- 230000008016 vaporization Effects 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 10
- QICQRRAHXUYAHB-UHFFFAOYSA-N benzene;formonitrile Chemical compound N#C.C1=CC=CC=C1 QICQRRAHXUYAHB-UHFFFAOYSA-N 0.000 claims description 8
- 230000006837 decompression Effects 0.000 claims description 8
- 238000005660 chlorination reaction Methods 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 2
- 239000002917 insecticide Substances 0.000 abstract 2
- 239000013078 crystal Substances 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PDNNQADNLPRFPG-UHFFFAOYSA-N N.[O] Chemical compound N.[O] PDNNQADNLPRFPG-UHFFFAOYSA-N 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 2
- CKAPSXZOOQJIBF-UHFFFAOYSA-N hexachlorobenzene Chemical compound ClC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl CKAPSXZOOQJIBF-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 235000011437 Amygdalus communis Nutrition 0.000 description 1
- MHXUIYGGILFLKW-UHFFFAOYSA-N N#CC#N.ClC=1C(=C(C(=C(C1)Cl)Cl)Cl)Cl Chemical compound N#CC#N.ClC=1C(=C(C(=C(C1)Cl)Cl)Cl)Cl MHXUIYGGILFLKW-UHFFFAOYSA-N 0.000 description 1
- 241000220304 Prunus dulcis Species 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 235000020224 almond Nutrition 0.000 description 1
- 238000005915 ammonolysis reaction Methods 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a production method of pentachlorobenzonitrile, which belongs to the field of the manufacturing of farm insecticides. The pentachlorobenzonitrile is white or almost white crystal powder in appearance, is an important intermediate of the farm insecticides, and has extremely wide purposes. The production method of the pentachlorobenzonitrile, which is provided by the invention, comprises the following steps: using toluene, ammonia, air or oxygen, chlorine, nitrogen and a catalyst as raw materials, first, preparing benzonitrile through an ammoxidation method in a fixed bed, and then, using the benzonitrile as a raw material, and producing the pentachlorobenzonitrile through a gas phase chlorination method, namely a process that a fluidized bed is used prior to the fixed bed. The production method has the advantages of simple process, high efficiency, low cost, short conversion time, no pollution, high yield and the like, and a qualified pentachlorobenzonitrile product can be produced.
Description
Affiliated technical field:
The invention belongs to agricultural chemicals and make the field, it is characterized in that relating to a kind of working method of pentachlorobenzene formonitrile HCN.
Background technology:
The pentachlorobenzene formonitrile HCN, another name pentachlorobenzene cyanogen; 2,3,4,5,6-pentachlorobenzene formonitrile HCN; 2,3,4,5, the 6-Perchlorobenzonitrile, outward appearance is white or off-white color crystalline powder, molecular formula is C
7Cl
5N, molecular weight are 275.34.The pentachlorobenzene formonitrile HCN is a kind of important pesticide intermediate, and purposes is very extensive, and its synthetic technology is more, and the present invention is wherein a kind of, and (toluene, molecular formula are C with toluene
7H
8, be a kind of colourless, with the volatile liquid of special aromatising flavour, one of aromatic hydrocarbons; Its a lot of character and benzene are very alike; But toxicity is a kind of industrial chemicals commonly used much smaller than benzene, can be used for making explosive, agricultural chemicals, phenylformic acid, cyanobenzene, dyestuff, synthetic resins and terylene etc.; It also is one of component of gasoline simultaneously, how from oil, to extract.) get cyanobenzene for raw material through ammonia oxygen legal system, the main points of this working method are: one, select or produce voluntarily appropriate catalyst for use; Two, will control suitable reaction temperature, temperature is difficult control in the ammonia oxidation strong exothermal reaction, facts have proved, when temperature was higher than 430 ℃, over oxidation took place, and the cyanobenzene selectivity is descended; Three, the air input of control ammonia; Ammonia is considered to cause in the oxidative ammonolysis high reactivity and principal element optionally; Facts have proved that best mole proportioning is a toluene vapour: ammonia: oxygen (or air)=1: 5-10: 30-35 makes cyanobenzene through fixed-bed reactor.(cyanobenzene, molecular formula are C with the cyanobenzene that makes
7H
5N, molecular weight are 103.12, and outward appearance is a colourless oil liquid, and the smell of almond is arranged, and fusing point is-12.8 ℃, and boiling point is 190.7 ℃, is slightly soluble in cold water, is dissolved in hot water, is soluble in ethanol, ether.) produce the pentachlorobenzene formonitrile HCN for raw material through the method for gas phase chlorination, the production main points of this method are: one, selecting suitable temperature and pressure, is that 0.01MPa-0.10Mpa is best through 180 ℃-220 ℃ of temperature, the pressure of testing this reaction of proof repeatedly; Two, select suitable air inlet than and the reaction times, be cyanobenzene vapour through the mole proportioning that facts have proved air input: chlorine: nitrogen=2-3: 4-9: 6-36 is for best, three, the selection appropriate catalyst, through fluidized-bed and fixed bed production pentachlorobenzene formonitrile HCN.Advantage of the present invention is: technology is simple, production cost is low, pollution-free, product yield is high and quality good.
Summary of the invention:
In order to overcome the defective that older production technique production cost is high, pollution is big, transformation time is long; The invention provides a kind of is that raw material is produced the pentachlorobenzene formonitrile HCN through oxidation proceses of ammonia, gas phase chlorination method with toluene; This method has that technology is simple, production cost is low, pollution-free, product yield is high and the measured advantage of matter, producing the raw material that this product uses has: toluene, ammonia, oxygen or air, nitrogen, chlorine and catalyzer.
The present invention can realize through following technical scheme:
A kind of method of suitability for industrialized production pentachlorobenzene formonitrile HCN is characterized in that being made up of following steps:
1, quantitative toluene is sent into vaporizer and vaporize, toluene vaporization back is taken out of vaporizer and in mixing tank, is mixed the back with ammonia by air and gets into fixed bed, and the mol ratio of three kinds of gas (vapour) body does; Toluene vapour: ammonia: air=1: 5-10: 30-35, temperature in the fixed bed is adjusted into 380 ℃-430 ℃, pressure is 0.05MPa-0.10Mpa; Add the BN-98 toluene prepared by ammoxidation cyanobenzene catalyzer that accounts for gas gross 0.2%; Reacted 0.3-0.5 hour, will react and send into collector after back gas decompression is lowered the temperature, after condensation, get products benzene formonitrile HCN liquid; The yield of product is 90%--95%, and purity is 99.5%.
2, cyanobenzene is sent into vaporizer and vaporize, cyanobenzene vaporization back is taken out of vaporizer and in mixing tank, is mixed the laggard fluidized-bed of going into chlorine by nitrogen, and the mol ratio of air input is a cyanobenzene: chlorine: nitrogen=2-3: 4-9: 6-36; Add the catalyst activity charcoal simultaneously; Quantity is the 0.2%-8% of an interior gas gross, and it is 0.01MPa-0.10Mpa that temperature in the fluidized-bed is transferred to 180 ℃-220 ℃, pressure, and reacted gas is sent into fixed bed; Keep the temperature and pressure identical with fluidized-bed; And add and add identical catalyst activity charcoal and the chlorine of fluidized-bed quantity, gas and chlorine behind the first set reaction are reacted again, after the reaction end; Mixed gas after the reaction in the fixed bed is sent into collector, and oven dry obtains the pentachlorobenzene formonitrile HCN after condensation.The yield of this reaction is 80%-95%, and product gas purity is 98%.Chlorine gets into fluidized-bed and fixed bed respectively in this reaction process; Adjust the load of two reactor drums through the quantity of two chlorine of adjustment entering; Thereby reduce the content of Perchlorobenzene; Through practice test, the hexachlorobenzene content that this reaction produces has only 40ppm-100ppm, is significantly less than state specified standards.
Fixed bed interior reaction temperature described in the above-mentioned steps 1 is 380 ℃-430 ℃, and pressure is 0.01MPa-0.11Mpa,
Temperature in the above-mentioned steps 2 in fluidized-bed and the fixed bed is that 180 ℃-220 ℃, pressure are 0.01MPa-0.10Mpa.
The invention has the beneficial effects as follows: it is raw material that a kind of toluene with large low price is provided; Produce the pentachlorobenzene formonitrile HCN through ammonia oxygen method, gas phase chlorination method, this working method has that technology is simple, efficient is high, and cost is low; Transformation time is short, pollution-free, can produce qualified pentachlorobenzene formonitrile HCN product.
Embodiment
Embodiment 1
Quantitative toluene is sent into vaporizer vaporize, toluene vaporization back is taken out of vaporizer and in mixing tank, is mixed the back with ammonia by air and gets into fixed bed, and the mol ratio of three kinds of gas (vapour) body does; Toluene vapour: ammonia: air=1: 5: 30, temperature in the fixed bed is adjusted into 380 ℃, pressure is 0.05MPa; Add the BN-98 toluene prepared by ammoxidation cyanobenzene catalyzer that accounts for gas gross 0.2%; Reacted 0.3-0.5 hour, will react and send into collector after back gas decompression is lowered the temperature, after condensation, get products benzene formonitrile HCN liquid; The yield of product is 90%--95%, and purity is 99.5%; Cyanobenzene is sent into vaporizer vaporizes, cyanobenzene vaporization back by nitrogen take out of vaporizer and with in mixing tank, mix the laggard fluidized-bed of going in chlorine, the mol ratio of air input is a cyanobenzene vapour: chlorine: nitrogen=2: 4: 6; Add the catalyst activity charcoal simultaneously; Quantity is 0.2% of an interior gas gross, and it is 0.01MPa that temperature in the fluidized-bed is transferred to 180 ℃, pressure, will react back gas and send into fixed bed; Keep the temperature and pressure identical with fluidized-bed; And add and add identical catalyst activity charcoal and the chlorine of fluidized-bed quantity, gas and chlorine behind the first set reaction are reacted again, after the reaction end; Mixed gas after the reaction in the fixed bed is sent into collector, and oven dry obtains the pentachlorobenzene formonitrile HCN after condensation.The yield of this reaction is 80%-95%, and product gas purity is 98%.
Embodiment 2
Quantitative toluene is sent into vaporizer vaporize, toluene vaporization back is taken out of vaporizer and in mixing tank, is mixed the back with ammonia by air and gets into fixed bed, and the mol ratio of three kinds of gas (vapour) body does; Toluene vapour: ammonia: air=1: 6: 31, temperature in the fixed bed is adjusted into 390 ℃, pressure is 0.06MPa; Add the BN-98 toluene prepared by ammoxidation cyanobenzene catalyzer that accounts for gas gross 0.2%; Reacted 0.3-0.5 hour, will react and send into collector after back gas decompression is lowered the temperature, after condensation, get products benzene formonitrile HCN liquid; The yield of product is 90%--95%, and purity is 99.5%; Cyanobenzene is sent into vaporizer vaporizes, cyanobenzene vaporization back by nitrogen take out of vaporizer and with in mixing tank, mix the laggard fluidized-bed of going in chlorine, the mol ratio of air input is a cyanobenzene vapour: chlorine: nitrogen=2.2: 5: 12; Add the catalyst activity charcoal simultaneously; Quantity is 0.6% of an interior gas gross, and it is 0.02Mpa that temperature in the fluidized-bed is transferred to 190 ℃, pressure, will react back gas and send into fixed bed; Keep the temperature and pressure identical with fluidized-bed; And add and add identical catalyst activity charcoal and the chlorine of fluidized-bed quantity, gas and chlorine behind the first set reaction are reacted again, after the reaction end; Mixed gas after the reaction in the fixed bed is sent into collector, and oven dry obtains the pentachlorobenzene formonitrile HCN after condensation.The yield of this reaction is 80%-95%, and product gas purity is 98%.
Embodiment 3
Quantitative toluene is sent into vaporizer vaporize, toluene vaporization back is taken out of vaporizer and in mixing tank, is mixed the back with ammonia by air and gets into fixed bed, and the mol ratio of three kinds of gas (vapour) body does; Toluene vapour ammonia: air=1: 7: 32, temperature in the fixed bed is adjusted into 400 ℃, pressure is 0.07MPa; Add the BN-98 toluene prepared by ammoxidation cyanobenzene catalyzer that accounts for gas gross 0.2%; Reacted 0.3-0.5 hour, will react and send into collector after back gas decompression is lowered the temperature, after condensation, get products benzene formonitrile HCN liquid; The yield of product is 90%--95%, and purity is 99.5%; Cyanobenzene is sent into vaporizer vaporizes, cyanobenzene vaporization back by nitrogen take out of vaporizer and with in mixing tank, mix the laggard fluidized-bed of going in chlorine, the mol ratio of air input is a cyanobenzene vapour: chlorine: nitrogen=2.4: 6: 18; Add the catalyst activity charcoal simultaneously; Quantity is 1% of an interior gas gross, and it is 0.03MPa that temperature in the fluidized-bed is transferred to 200 ℃, pressure, will react back gas and send into fixed bed; Keep the temperature and pressure identical with fluidized-bed; And add and add identical catalyst activity charcoal and the chlorine of fluidized-bed quantity, gas and chlorine behind the first set reaction are reacted again, after the reaction end; Mixed gas after the reaction in the fixed bed is sent into collector, and oven dry obtains the pentachlorobenzene formonitrile HCN after condensation.The yield of this reaction is 80%-95%, and product gas purity is 98%.
Embodiment 4
Quantitative toluene is sent into vaporizer vaporize, toluene vaporization back is taken out of vaporizer and in mixing tank, is mixed the back with ammonia by air and gets into fixed bed, and the mol ratio of three kinds of gas (vapour) body does; Toluene vapour: ammonia: air=1: 8: 33, temperature in the fixed bed is adjusted to 410 ℃, pressure is 0.08MPa; Add the BN-98 toluene prepared by ammoxidation cyanobenzene catalyzer that accounts for gas gross 0.2%; Reacted 0.3-0.5 hour, will react and send into collector after back gas decompression is lowered the temperature, after condensation, get products benzene formonitrile HCN liquid; The yield of product is 90%--95%, and purity is 99.5%; Cyanobenzene is sent into vaporizer vaporizes, cyanobenzene vaporization back by nitrogen take out of vaporizer and with in mixing tank, mix the laggard fluidized-bed of going in chlorine, the mol ratio of air input is a cyanobenzene vapour: chlorine: nitrogen=2.6: 7: 24; Add the catalyst activity charcoal simultaneously; Quantity is 1.5% of an interior gas gross, and it is 0.04MPa that temperature in the fluidized-bed is transferred to 210 ℃, pressure, will react back gas and send into fixed bed; Keep the temperature and pressure identical with fluidized-bed; And add and add identical catalyst activity charcoal and the chlorine of fluidized-bed quantity, gas and chlorine behind the first set reaction are reacted again, after the reaction end; Mixed gas after the reaction in the fixed bed is sent into collector, and oven dry obtains the pentachlorobenzene formonitrile HCN after condensation.The yield of this reaction is 80%-95%, and product gas purity is 98%.
Embodiment 5
Quantitative toluene is sent into vaporizer vaporize, toluene vaporization back is taken out of vaporizer and in mixing tank, is mixed the back with ammonia by air and gets into fixed bed, and the mol ratio of three kinds of gas (vapour) body does; Toluene vapour: ammonia: air=1: 9: 34, temperature in the fixed bed is adjusted into 420 ℃, pressure is 0.09MPa; Add the BN-98 toluene prepared by ammoxidation cyanobenzene catalyzer that accounts for gas gross 0.2%; Reacted 0.3-0.5 hour, will react and send into collector after back gas decompression is lowered the temperature, after condensation, get products benzene formonitrile HCN liquid; The yield of product is 90%--95%, and purity is 99.5%; Cyanobenzene is sent into vaporizer vaporizes, cyanobenzene vaporization back by nitrogen take out of vaporizer and with in mixing tank, mix the laggard fluidized-bed of going in chlorine, the mol ratio of air input is a cyanobenzene vapour: chlorine: nitrogen=2.8: 8: 30; Add the catalyst activity charcoal simultaneously; Quantity is 1.9% of an interior gas gross, and it is 0.05MPa that temperature in the fluidized-bed is transferred to 220 ℃, pressure, will react back gas and send into fixed bed; Keep the temperature and pressure identical with fluidized-bed; And add and add identical catalyst activity charcoal and the chlorine of fluidized-bed quantity, gas and chlorine behind the first set reaction are reacted again, after the reaction end; Mixed gas after the reaction in the fixed bed is sent into collector, and oven dry obtains the pentachlorobenzene formonitrile HCN after condensation.The yield of this reaction is 80%-95%, and product gas purity is 98%.
Embodiment 6
Quantitative toluene is sent into vaporizer vaporize, toluene vaporization back is taken out of vaporizer and in mixing tank, is mixed the back with ammonia by air and gets into fixed bed, and the mol ratio of three kinds of gas (vapour) body does; Toluene vapour: ammonia: air=1: 10: 35, temperature in the fixed bed is adjusted into 430 ℃, pressure is 0.10Mpa; Add the BN-98 toluene prepared by ammoxidation cyanobenzene catalyzer that accounts for gas gross 0.2%; Reacted 0.3-0.5 hour, will react and send into collector after back gas decompression is lowered the temperature, after condensation, get products benzene formonitrile HCN liquid; The yield of product is 90%--95%, and purity is 99.5%; Cyanobenzene is sent into vaporizer vaporizes, cyanobenzene vaporization back by nitrogen take out of vaporizer and with in mixing tank, mix the laggard fluidized-bed of going in chlorine, the mol ratio of air input is a cyanobenzene vapour: chlorine: nitrogen=3: 9: 36; Add the catalyst activity charcoal simultaneously; Quantity is 2.4% of an interior gas gross, and it is 0.06Mpa that temperature in the fluidized-bed is transferred to 220 ℃, pressure, will react back gas and send into fixed bed; Keep the temperature and pressure identical with fluidized-bed; And add and add identical catalyst activity charcoal and the chlorine of fluidized-bed quantity, gas and chlorine behind the first set reaction are reacted again, after the reaction end; Mixed gas after the reaction in the fixed bed is sent into collector, and oven dry obtains the pentachlorobenzene formonitrile HCN after condensation.The yield of this reaction is 80%-95%, and product gas purity is 98%.
Claims (5)
1. the working method of a pentachlorobenzene formonitrile HCN, it is characterized in that: with toluene, ammonia, oxygen or air, nitrogen, chlorine and catalyzer is raw material, obtains finished product through following steps.
2. the working method of a kind of pentachlorobenzene formonitrile HCN according to claim 1, the characteristic of its first step is: quantitative toluene is sent into vaporizer vaporize, toluene vaporization back is taken out of vaporizer and in mixing tank, is mixed the back with ammonia by air and gets into fixed bed; The mol ratio of three kinds of gas (vapour) body does; Toluene vapour: ammonia: air=1: 5-10: 30-35, temperature in the fixed bed is adjusted into 380 ℃-430 ℃, pressure is 0.05MPa-0.10Mpa; Add the BN-98 toluene prepared by ammoxidation cyanobenzene catalyzer that accounts for gas gross 0.2%; Reacted 0.3-0.5 hour, will react and send into collector after back gas decompression is lowered the temperature, after condensation, get products benzene formonitrile HCN liquid; The yield of product is 90%--95%, and purity is 99.5%.
3. the working method of a kind of pentachlorobenzene formonitrile HCN according to claim 1; The characteristic in its second step is: cyanobenzene is sent into vaporizer vaporize, cyanobenzene vaporization back is taken out of vaporizer and in mixing tank, is mixed the laggard fluidized-bed of going into chlorine by nitrogen, and the mol ratio of air input is a cyanobenzene vapour: chlorine: nitrogen=2-3: 4-9: 6-36; Add the catalyst activity charcoal simultaneously; Quantity is the 0.2%-8% of an interior gas gross, and it is 0.01MPa-0.10Mpa that temperature in the fluidized-bed is transferred to 180 ℃-220 ℃, pressure, will react back gas and send into fixed bed; Keep the temperature and pressure identical with fluidized-bed; And add and add identical catalyst activity charcoal and the chlorine of fluidized-bed quantity, gas and chlorine behind the first set reaction are reacted again, after the reaction end; Mixed gas after the reaction in the fixed bed is sent into collector, and oven dry obtains the pentachlorobenzene formonitrile HCN after condensation.The yield of this reaction is 80%-95%, and product gas purity is 98%.
4. the fixed bed interior reaction temperature described in the aforesaid right requirement 2 is 380 ℃-430 ℃, and pressure is 0.01MPa-0.11Mpa,
5. to require in 3 the temperature in the fluidized-bed and fixed bed be that 180 ℃-220 ℃, pressure are 0.01MPa-0.10Mpa to aforesaid right.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107597091A (en) * | 2017-09-25 | 2018-01-19 | 江苏苏利精细化工股份有限公司 | A kind of production method of high-purity Perchlorobenzonitrile |
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