CN107511155A - A kind of catalyst for preparing Bravo and its preparation method and application - Google Patents
A kind of catalyst for preparing Bravo and its preparation method and application Download PDFInfo
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- CN107511155A CN107511155A CN201610425142.1A CN201610425142A CN107511155A CN 107511155 A CN107511155 A CN 107511155A CN 201610425142 A CN201610425142 A CN 201610425142A CN 107511155 A CN107511155 A CN 107511155A
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- catalyst
- bravo
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- chloride
- activated carbon
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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
- B01J27/06—Halogens; Compounds thereof
- B01J27/138—Halogens; Compounds thereof with alkaline earth metals, magnesium, beryllium, zinc, cadmium or mercury
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/30—Preparation of carboxylic acid nitriles by reactions not involving the formation of cyano groups
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
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Abstract
The present invention relates to a kind of catalyst for preparing Bravo and its preparation method and application, makees carrier, main active substances FeCl with activated carbon3, auxiliary active agent is at least one of Cu and Ca chloride and Na, K or Cs chloride, wherein：Fe, Cu, Ca mol ratio are 1:0.1‑0.8:0.1 0.9, Fe and Na, K or Cs mol ratio are 1:0.01 0.3, main active substances and auxiliary active agent account for 5 20wt% of catalyst total amount, and the catalyst can use in Bravo high-temperature chlorination fluid bed is prepared by isophthalodinitrile.Compared with prior art, the advantages of present invention has Bravo high income, and content is high, and catalyst preparation process is simple, catalyst cost is relatively low, long lifespan, available for industrial production.
Description
Technical field
The present invention relates to a kind of pesticide catalyst, more particularly, to a kind of catalyst for preparing Bravo and preparation method thereof
And application.
Background technology
Bravo is a kind of efficient, low toxicity, wide spectrum, the protective fungicide of low-residual, is widely used in agricultural and woods
The fungal disease preventing and treating of industry, using many especially on the industrial crops such as vegetables, fruit.Can be right according to Japanese data report Bravo
52 kinds of diseases of 30 various crops have prevention effect.In addition, Bravo also has important use in mould proof industrial circle,
Such as manufacture mildew resistant paint, mould proof wallpaper, electrical equipment is mould proof, Pi Ping, timber etc. it is mould proof.The production scale of Bravo at home is continuous
Expand, it has also become one of excellent pesticide species of large-tonnage in the world.
Bravo be as isophthalodinitrile in fluid bed by high-efficiency low-toxicity, broad-spectrum sterilization class weight obtained by catalytic chlorination
Want Pesticidal products.The chlorination catalyst used at present is substantially used from Japanese import.Japanese catalyst is urged relative to domestic
Agent is due to its steady quality, and high income, hexachloro-benzene control is preferable, so dosage is larger, but its supply is limited, and price
It is higher, often restrict the production of the product.
The content of the invention
The purpose of the present invention is exactly for the problem such as overcome domestic catalyst poor activity, poor selectivity, conversion ratio low, there is provided
A kind of catalyst for preparing Bravo and its preparation method and application.Using this catalyst, good, the high conversion rate of selectivity, system
Standby technique is simple, and catalyst cost is relatively low, long lifespan.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of catalyst for preparing Bravo, carrier, main active substances FeCl are made with activated carbon3, auxiliary activity thing
Matter is at least one of Cu and Ca chloride and Na, K or Cs chloride, wherein：Fe, Cu, Ca mol ratio are 1:
0.1-0.8:0.1-0.9, Fe and Na, K or Cs mol ratio are 1:0.01-0.3, main active substances and auxiliary active agent account for
The 5-20wt% of catalyst total amount.
Preferably, activated carbon is the cocoanut active charcoal of 15-60 mesh.
Preferably, Fe, Cu, Ca mol ratio are 1:0.4-0.6:0.5-0.7.
Preferably, Fe and Na, K or Cs mol ratio are 1:0.1-0.2.
Preferably, main active substances and auxiliary active agent account for the 10-15wt% of catalyst total amount.
The preparation method of the catalyst of Bravo is prepared, using following steps：
(1) chloride or the salt watery hydrochloric acid that will form each component element of main active substances and auxiliary active agent are molten
Solution forms solution,
(2) activated carbon is poured into solution, activated carbon and solution weight ratio are 1:1-1:5, using digestion seasoning, heating
The catalyst for obtaining preparing Bravo is further dried to 90 DEG C of digestions to doing in stirring at 120 DEG C.
The catalyst of Bravo is prepared, can be made in Bravo high-temperature chlorination fluid bed is prepared by isophthalodinitrile
With.
Reaction product is reclaimed from reactor outlet mixture using the method for cold trapping.Specific method is as follows：Will reaction
Device exports gaseous mixture and direct cools to the temperature that reaction product separates out into solid by thin-walled cooler, makes product in thin-walled cooling
Separated out in device to reclaim product therein.
Compared with prior art, the present invention has advantages below：
1st, for the present invention by being impregnated under higher temperature, one side higher temperature is advantageous to absorption in activated carbon duct
The desorption of adsorbed gas, be on the other hand advantageous to mass transfer of the dipping solution in activated carbon duct, be easy to the gas in duct
Discharge, and then all channel surfaces inside activated carbon is obtained modification, improve the performance of the catalyst.
2nd, high income.Compared with existing technology, invention increases alkali metal and other metallic elements.Using this hair
Bright provided catalyst feed stock conversion is higher, and the selectivity and yield of product are all higher, can further reduce and be produced into
This, so the technology has relatively good application value.
A kind of new catalyst for preparing Bravo provided by the present invention, feed stock conversion is high, the selectivity and receipts of product
Rate is all higher, can further reduce production cost, and raw material selection is extensive, and preparation method is simple, and the present invention, which has, preferably to be pushed away
Wide application value.
Embodiment
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
Catalyst preparation
By 165gFeCl3, 94.5gCuCl2,89gCaCl2 and 15gCsCl are added to containing 50ml concentrated hydrochloric acids together
In the solution of 1450ml distilled water, add the cocoanut active charcoal of 1500g 15-60 mesh, agitating and heating, 90 DEG C of digestions to dry, then at
Dried 24 hours at 120 DEG C, produce required catalyst.
Isophthalodinitrile chlorination
Obtained catalyst 200g is filled into fluidized-bed reactor, is passed through nitrogen at 120 DEG C, gas velocity 0.11m/s,
Dry 4 hours, chlorine is passed through at 260 DEG C, 40g/h is activated 6 hours, by isophthalodinitrile：Chlorine：Nitrogen=1:2.5：
The ratio mixed gas of 2.5 (mass ratioes) is passed through reactor, and temperature control is in 300 DEG C of reactions, you can Bravo is obtained, Bravo
Molar yield 98.1%.
Embodiment 2
Catalyst preparation
By 165gFeCl3, 108gCuCl2,89gCaCl2 and 7.5gKCl are added to containing 50ml concentrated hydrochloric acids together
In the solution of 1450ml distilled water, add the cocoanut active charcoal of 1500g 15-60 mesh, agitating and heating, 90 DEG C of digestions to dry, then at
Dried 24 hours at 120 DEG C, produce required catalyst.
Isophthalodinitrile chlorination
Obtained catalyst 200g is filled into fluidized-bed reactor, is passed through nitrogen at 120 DEG C, gas velocity 0.11m/s,
Dry 4 hours, chlorine is passed through at 260 DEG C, 40g/h is activated 6 hours, by isophthalodinitrile：Chlorine：Nitrogen=1:2.5：
The ratio mixed gas of 2.5 (mass ratioes) is passed through reactor, and temperature control is in 300 DEG C of reactions, you can Bravo is obtained, Bravo
Molar yield 98.4%.
Embodiment 3
Catalyst preparation
By 165gFeCl3, 81gCuCl2,78gCaCl2 and 6gNaCl are added to the 1450ml containing 50ml concentrated hydrochloric acids together
In the solution of distilled water, the cocoanut active charcoal of 1500g 15-60 mesh is added, agitating and heating, 90 DEG C of digestions are to doing, then at 120 DEG C
Lower drying 24 hours, produce required catalyst.
Isophthalodinitrile chlorination
Obtained catalyst 200g is filled into fluidized-bed reactor, is passed through nitrogen at 120 DEG C, gas velocity 0.11m/s,
Dry 4 hours, chlorine is passed through at 260 DEG C, 40g/h is activated 6 hours, by isophthalodinitrile：Chlorine：Nitrogen=1:2.5：
The ratio mixed gas of 2.5 (mass ratioes) is passed through reactor, and temperature control is in 300 DEG C of reactions, you can obtains Bravo, Bravo
Molar yield 98.3%.
Embodiment 4
Catalyst preparation
By 132gFeCl3, 64.8gCuCl2,62.4gCaCl2,6gKCl and 4.8NaCl are added to dense containing 50ml together
In the solution of the 1450ml distilled water of hydrochloric acid, the cocoanut active charcoal of 1500g 15-60 mesh is added, agitating and heating, 90 DEG C of digestions are extremely
It is dry, dried 24 hours at 120 DEG C, produce required catalyst.
Isophthalodinitrile chlorination
Obtained catalyst 200g is filled into fluidized-bed reactor, is passed through nitrogen at 120 DEG C, gas velocity 0.11m/s,
Dry 4 hours, chlorine is passed through at 260 DEG C, 40g/h is activated 6 hours, by isophthalodinitrile：Chlorine：Nitrogen=1:2.5：
The ratio mixed gas of 2.5 (mass ratioes) is passed through reactor, and temperature control is in 300 DEG C of reactions, you can Bravo is obtained, Bravo
Molar yield 97.8%.
Embodiment 5
Catalyst preparation
By 79.2gFeCl3, 38.9gCuCl2,37.4gCaCl2,3.6gKCl and 2.9NaCl are added to containing 50ml together
In the solution of the 1450ml distilled water of concentrated hydrochloric acid, the cocoanut active charcoal of 1500g 15-60 mesh, agitating and heating, 90 DEG C of digestions are added
To dry, dry 24 hours at 120 DEG C, the catalyst required for producing.
Isophthalodinitrile chlorination
Obtained catalyst 200g is filled into fluidized-bed reactor, is passed through nitrogen at 120 DEG C, gas velocity 0.11m/s,
Dry 4 hours, chlorine is passed through at 260 DEG C, 40g/h is activated 6 hours, by isophthalodinitrile：Chlorine：Nitrogen=1:2.5：
The ratio mixed gas of 2.5 (mass ratioes) is passed through reactor, and temperature control is in 300 DEG C of reactions, you can Bravo is obtained, Bravo
Molar yield 96.0%.
Embodiment 6
Catalyst preparation
By 165gFeCl3, 67.5gCuCl2,78gCaCl2,10CsCl and 6gNaCl are added to containing the dense salt of 50ml together
In the solution of the 1450ml distilled water of acid, add the cocoanut active charcoal of 1500g 15-60 mesh, agitating and heating, 90 DEG C of digestions to dry,
Dried 24 hours at 120 DEG C, produce required catalyst.
Isophthalodinitrile chlorination
Obtained catalyst 200g is filled into fluidized-bed reactor, nitrogen, gas velocity 0.11m/ are passed through at 120 DEG C
S, dry 4 hours, chlorine is passed through at 260 DEG C, 40g/h is activated 6 hours, by isophthalodinitrile：Chlorine：Nitrogen=1:2.5：
The ratio mixed gas of 2.5 (mass ratioes) is passed through reactor, and temperature control is in 300 DEG C of reactions, you can Bravo is obtained, Bravo
Molar yield 98.4%.
Embodiment 7
A kind of catalyst for preparing Bravo, carrier, main active substances FeCl are made with the cocoanut active charcoal of 15 mesh3,
Auxiliary active agent be Cu and Ca chloride and Na chloride, wherein：Fe, Cu, Ca mol ratio are 1:0.1:0.1,
Fe and Na mol ratio is 1:0.01, main active substances and auxiliary active agent account for the 5wt% of catalyst total amount.
The preparation method of the catalyst of Bravo is prepared, using following steps：
(1) chloride or the salt watery hydrochloric acid that will form each component element of main active substances and auxiliary active agent are molten
Solution forms solution,
(2) activated carbon is poured into solution, activated carbon and solution weight ratio are 1:1, using digestion seasoning, heating stirring
To 90 DEG C of digestions to doing, the catalyst for obtaining preparing Bravo is further dried at 120 DEG C, can be by isophthalic diformazan
Prepared by nitrile uses in Bravo high-temperature chlorination fluid bed.
Embodiment 8
A kind of catalyst for preparing Bravo, carrier, main active substances FeCl are made with the cocoanut active charcoal of 20 mesh3,
Auxiliary active agent be Cu and Ca chloride and Na, K chloride, wherein：Fe, Cu, Ca mol ratio are 1:0.4:
0.5, Fe with Na, K mol ratio is 1:0.1, main active substances and auxiliary active agent account for the 10wt% of catalyst total amount.
The preparation method of the catalyst of Bravo is prepared, using following steps：
(1) chloride or the salt watery hydrochloric acid that will form each component element of main active substances and auxiliary active agent are molten
Solution forms solution,
(2) activated carbon is poured into solution, activated carbon and solution weight ratio are 1:2, using digestion seasoning, heating stirring
To 90 DEG C of digestions to doing, the catalyst for obtaining preparing Bravo is further dried at 120 DEG C, can be by isophthalic diformazan
Prepared by nitrile uses in Bravo high-temperature chlorination fluid bed.
Embodiment 9
A kind of catalyst for preparing Bravo, carrier, main active substances FeCl are made with the cocoanut active charcoal of 30 mesh3,
Auxiliary active agent be Cu and Ca chloride and K chloride, wherein：Fe, Cu, Ca mol ratio are 1:0.6:0.7, Fe
Mol ratio with K is 1:0.2, main active substances and auxiliary active agent account for the 15wt% of catalyst total amount.
The preparation method of the catalyst of Bravo is prepared, using following steps：
(1) chloride or the salt watery hydrochloric acid that will form each component element of main active substances and auxiliary active agent are molten
Solution forms solution,
(2) activated carbon is poured into solution, activated carbon and solution weight ratio are 1:3, using digestion seasoning, heating stirring
To 90 DEG C of digestions to doing, the catalyst for obtaining preparing Bravo is further dried at 120 DEG C, can be by isophthalic diformazan
Prepared by nitrile uses in Bravo high-temperature chlorination fluid bed.
Embodiment 10
A kind of catalyst for preparing Bravo, carrier, main active substances FeCl are made with the cocoanut active charcoal of 60 mesh3,
Auxiliary active agent be Cu and Ca chloride and Cs chloride, wherein：Fe, Cu, Ca mol ratio are 1:0.8:0.9,
Fe and Cs mol ratio is 1:0.3, main active substances and auxiliary active agent account for the 20wt% of catalyst total amount.
The preparation method of the catalyst of Bravo is prepared, using following steps：
(1) chloride or the salt watery hydrochloric acid that will form each component element of main active substances and auxiliary active agent are molten
Solution forms solution,
(2) activated carbon is poured into solution, activated carbon and solution weight ratio are 1:5, using digestion seasoning, heating stirring
To 90 DEG C of digestions to doing, the catalyst for obtaining preparing Bravo is further dried at 120 DEG C, can be by isophthalic diformazan
Prepared by nitrile uses in Bravo high-temperature chlorination fluid bed.
Using new catalyst provided by the present invention and corresponding chlorination method, feed stock conversion is high, the choosing of product
Selecting property and yield are all higher, can further reduce production cost.
General principle, principal character and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, various changes and modifications of the present invention are possible without departing from the spirit and scope of the present invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent defines.
Claims (8)
1. a kind of catalyst for preparing Bravo, it is characterised in that the catalyst makees carrier with activated carbon, and main active substances are
FeCl3, auxiliary active agent is at least one of Cu and Ca chloride and Na, K or Cs chloride, wherein：Fe、Cu、
Ca mol ratio is 1:0.1-0.8:0.1-0.9, Fe and Na, K or Cs mol ratio are 1:0.01-0.3, main active substances and
Auxiliary active agent accounts for the 5-20wt% of catalyst total amount.
2. a kind of catalyst for preparing Bravo according to claim 1, it is characterised in that described activated carbon is 15-
The cocoanut active charcoal of 60 mesh.
3. a kind of catalyst for preparing Bravo according to claim 1, it is characterised in that Fe, Cu, Ca mol ratio is
1:0.4-0.6:0.5-0.7。
4. a kind of catalyst for preparing Bravo according to claim 1, it is characterised in that Fe and Na, K or Cs mole
Than for 1:0.1-0.2.
A kind of 5. catalyst for preparing Bravo according to claim 1, it is characterised in that described main active substances
And auxiliary active agent accounts for the 10-15wt% of catalyst total amount.
6. the preparation method of the catalyst as claimed in claim 1 for preparing Bravo, it is characterised in that this method is using following
Step：
(1) chloride or salt diluted hydrochloric acid dissolution shape of each component element of main active substances and auxiliary active agent will be formed
Into solution,
(2) activated carbon is poured into solution, activated carbon and solution weight ratio are 1:1-1:5, using digestion seasoning, heating stirring
It is evaporated to liquid, further drying to obtain prepares the catalyst of Bravo.
A kind of 7. preparation method of catalyst for preparing Bravo according to claim 6, it is characterised in that step (2)
Then middle heating stirring is dried to 90 DEG C of digestions to doing at 120 DEG C.
8. the catalyst as claimed in claim 1 for preparing Bravo is preparing Bravo high-temperature chlorination by isophthalodinitrile
Applied in fluid bed.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610425142.1A CN107511155B (en) | 2016-06-15 | 2016-06-15 | Catalyst for preparing chlorothalonil and preparation method and application thereof |
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| CN201610425142.1A CN107511155B (en) | 2016-06-15 | 2016-06-15 | Catalyst for preparing chlorothalonil and preparation method and application thereof |
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Cited By (3)
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| CN108329235A (en) * | 2018-03-02 | 2018-07-27 | 天津赛普泰克科技有限公司 | A kind of process producing high-purity Bravo |
| CN110845366A (en) * | 2019-12-03 | 2020-02-28 | 万华化学集团股份有限公司 | Preparation method and preparation system of chlorothalonil |
| CN116199601A (en) * | 2023-05-06 | 2023-06-02 | 山东大成生物化工有限公司 | Refining and purifying process of high-content chlorothalonil |
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| CN116199601A (en) * | 2023-05-06 | 2023-06-02 | 山东大成生物化工有限公司 | Refining and purifying process of high-content chlorothalonil |
| CN116199601B (en) * | 2023-05-06 | 2023-08-11 | 山东大成生物化工有限公司 | Refining and purifying process of high-content chlorothalonil |
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