CN107056650A - The preparation of high-purity Bravo - Google Patents
The preparation of high-purity Bravo Download PDFInfo
- Publication number
- CN107056650A CN107056650A CN201610915081.7A CN201610915081A CN107056650A CN 107056650 A CN107056650 A CN 107056650A CN 201610915081 A CN201610915081 A CN 201610915081A CN 107056650 A CN107056650 A CN 107056650A
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- CN
- China
- Prior art keywords
- bravo
- chlorine
- isophthalodinitrile
- nitrogen
- vaporizer
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- 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.)
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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
Abstract
It is to put into the isophthalodinitrile of metering in vaporizer to be vaporized the invention discloses the preparation method of high-purity Bravo, isophthalodinitrile takes vaporizer out of through nitrogen and sequentially enters fluid bed and fixed bed equipped with special chlorination catalyst after being mixed in mixing with chlorine after vaporizing is reacted.The mol ratio of air inflow is isophthalodinitrile：Nitrogen：Chlorine=1:2‑5:45, the reaction temperature of fluid bed and fixed bed is controlled at 340-350 DEG C respectively, the 0.005MP of pressure 0.002, and after reaction terminates, reaction mixture gas feeding collector can obtain Bravo after condensation is dried.
Description
Technical field
The invention belongs to chemical production technical field, the preparation method of being related to protection of property fungicide chlorothalonil, and in particular to
The preparation of high-purity Bravo.
Background technology
Bravo chemical name is daconil M（The benzene dicarbonitrile of 2,4,5,6 one tetrachloro one 1,3 one）Sterling is white
Tasteless powder, 350 DEG C of boiling point, 250-251 DEG C of fusing point is slightly soluble in water, is dissolved in dimethylbenzene and acetone and other organic solvent.Former powder contains
Composition 96% is imitated, outward appearance is buff powder, slightly pungent odor, to acid, alkali, UV stable.Low toxicity, to lagophthalmos eyeball and angle
Film has obvious stimulation effect, can produce the opacity of the cornea, and irreversible, but does not have such a effect to eye.To a small number of fells
Skin has stimulation.Bravo is that a kind of non-internal-absorting wide-spectrum bactericide has prevention effect to various crop fungal disease.Energy
Have an effect, contain with the protein knot containing cysteine in the enzyme body with the glyceraldehyde 3-phosphate dehydro-genase in fungal cell,
The vigor of destructive enzyme, makes the metabolism of fungal cell be destroyed and loss of life power.The main function of Bravo is to prevent plant
Encroached on by fungi.Encroached on by germ in plant, after germ enters in plant, bactericidal action root is small.Bravo does not have
There is uptake and translocation effect, will not be absorbed from the root system at spray position and plant.Bravo has good stick together in plant surface
Property, it is difficult to be washed away by rainwater etc., therefore with longer drug effect phase, under conventional amount used, general drug effect phase about 7~l0d.Pass through
Tired agent or dust agent smog or the sedimentation of ultra tiny dust fine particle are attached to plant surface, play drug action, it is adaptable to protect
Shield ground.
Hexachloro-benzene is the impurity produced by superchlorination in Bravo building-up process, and abbreviation HCB is a kind of organic dirt of persistence
Contaminate thing.As countries in the world become better and approaching perfection day by day to environmental protection, to the requirement more and more higher of HCB in Bravo, according to new FAO
HCB in standard, Bravo is required to control in 40ppm once, and European and American areas is then required to control in 20ppm once, part state
Family then requires control in 10ppm once.
The conventional synthetic method of Bravo send into vaporizer for m-dicyanobenzene after melting and vaporized or directly and fraction
（N2）Reactor is carried out by nozzle atomization.Chlorine is mixed after drying and preheating with gaseous state m-dicyanobenzene, and nitrogen is used as carrier gas
Vaporize or be atomized for m-dicyanobenzene and regulation reactant concentration.Reactor uses fluid bed or other forms, gas after reaction
Through entering trap, Bravo, which is sublimated, to be separated out and sends out as product, yield 90% by continuous.Tail gas is mainly chlorine, hydrogen chloride and nitrogen
Gas, can partly circulate or all remove tail gas recovery and processing system.Also can use by liquid carbon tetrachloride spray into trap in, with
After reaction gas contact, Bravo is sublimated precipitation.Carbon tetrachloride is then vaporized, and is together discharged with tail gas, through being cooled further to -6 DEG C,
Carbon tetrachloride condensation cycle is used.
The production method for a kind of low hexachlorobenzene content chlorothalonil that CN200610048783.6 is proposed, using fluid bed and admittedly
The method that fixed bed is combined, while leading to the technique of chlorine using two steps, HCB contents can be less than substantially in its Bravo produced
40ppm requirement, but its production process leads to the technique of chlorine using two steps, causes technology controlling and process point many, actual production operation is tired
Difficulty, while not only the consumption of chlorine is big, and production post processing workload is also than larger, large-scale production more difficulty.
The Bravo production technology that CN201110076389.4 is proposed is similar with CN200610048783.6, equally adopts
The mode for taking two steps to lead to chlorine carries out production Bravo, and the defect existed is that logical chlorine dose is also larger.
The scheme that CN201410740625.1 is proposed is to use modified cocoanut active charcoal for catalyst, and same takes two steps
The mode of logical chlorine is produced, and the shortcoming existed is that logical chlorine control point is more, and logical chlorine dose is excessive, and exhaust aftertreatment workload is big.
The content of the invention
The present invention is directed to the deficiency of existing process technology, and the logical chlorine mode of the original multiple-hearth of improvement produces low hexachlorobenzene and contained
Amount, the Bravo active compound of high-purity, its yield reach more than 97%, and content reaches more than 99.5%, HCB≤10ppm.
The present invention is achieved by the following technical programs.
The preparation method of high-purity Bravo is to put into the isophthalodinitrile of metering in vaporizer to be vaporized, isophthalic
Vaporizer is taken out of through nitrogen and sequentially entered with chlorine after being mixed in mixing equipped with special chlorination catalyst after dimethoxy nitrile vaporization
Fluid bed and fixed bed reacted.The mol ratio of air inflow is isophthalodinitrile：Nitrogen：Chlorine=1:2-5:4-5, fluidisation
The reaction temperature of bed and fixed bed is controlled at 340-350 DEG C respectively, and pressure 0.002-0.005MP after reaction terminates, reacts mixed
Close pneumatic transmission and enter collector, Bravo is can obtain after condensation is dried.
Due to the utilization of above-mentioned technical proposal, the present invention has following advantages compared with prior art：
The low content hexachloro-benzene of the present invention, the preparation of high-purity Bravo, by the way of chlorine is once led to, in actual production process
Reduce logical chlorine control point, technique and operate practical, step is simple, its yield reaches more than 97%, content reach 99.5% with
On, HCB≤10ppm.
Embodiment
Embodiment 1
The isophthalodinitrile of metering is put into vaporizer and is vaporized, vaporizer is taken out of through nitrogen after isophthalodinitrile vaporization
And sequentially enter fluid bed and fixed bed equipped with special chlorination catalyst after being mixed in mixing with chlorine and reacted.Air inlet
The mol ratio of amount is isophthalodinitrile：Nitrogen：Chlorine=1:2.5:4.2, the reaction temperature of fluid bed and fixed bed is controlled respectively
342 DEG C, pressure 0.003MP, after reaction terminates, reaction mixture gas feeding collector obtains Bravo after condensation is dried, received
Rate is 97.2%, and content is that 99.5%, HCB is 9.5ppm.
Embodiment 2
The isophthalodinitrile of metering is put into vaporizer and is vaporized, vaporizer is taken out of through nitrogen after isophthalodinitrile vaporization
And sequentially enter fluid bed and fixed bed equipped with special chlorination catalyst after being mixed in mixing with chlorine and reacted.Air inlet
The mol ratio of amount is isophthalodinitrile：Nitrogen：Chlorine=1:3:4.5, the reaction temperature of fluid bed and fixed bed is controlled respectively
345 DEG C, pressure 0.003MP, after reaction terminates, reaction mixture gas feeding collector obtains Bravo after condensation is dried, received
Rate is 97.3%, and content is that 99.6%, HCB is 9ppm.
Embodiment 3
The isophthalodinitrile of metering is put into vaporizer and is vaporized, vaporizer is taken out of through nitrogen after isophthalodinitrile vaporization
And sequentially enter fluid bed and fixed bed equipped with special chlorination catalyst after being mixed in mixing with chlorine and reacted.Air inlet
The mol ratio of amount is isophthalodinitrile：Nitrogen：Chlorine=1:4:5, the reaction temperature of fluid bed and fixed bed is controlled 345 respectively
DEG C, pressure 0.004MP, after reaction terminates, reaction mixture gas feeding collector obtains Bravo, yield after condensation is dried
For 97.2%, content is that 99.7%, HCB is 8ppm.
Claims (3)
1. claim
The preparation of high-purity Bravo, is vaporized, isophthalic it is characterized in that the isophthalodinitrile of metering is put into vaporizer
Vaporizer is taken out of through nitrogen and sequentially entered with chlorine after being mixed in mixing equipped with special chlorination catalyst after dimethoxy nitrile vaporization
Fluid bed and fixed bed reacted.
2. the mol ratio of air inflow is isophthalodinitrile：Nitrogen：Chlorine=1:2-5:The reaction temperature of 4-5, fluid bed and fixed bed
Control respectively at 340-350 DEG C, pressure 0.002-0.005MP is reacted after terminating, reaction mixture gas feeding collector, through supercooling
Coagulate and can obtain Bravo after drying.
3. claim 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610915081.7A CN107056650A (en) | 2016-10-20 | 2016-10-20 | The preparation of high-purity Bravo |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610915081.7A CN107056650A (en) | 2016-10-20 | 2016-10-20 | The preparation of high-purity Bravo |
Publications (1)
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| CN107056650A true CN107056650A (en) | 2017-08-18 |
Family
ID=59617255
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610915081.7A Pending CN107056650A (en) | 2016-10-20 | 2016-10-20 | The preparation of high-purity Bravo |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109265365A (en) * | 2018-12-06 | 2019-01-25 | 江苏新河农用化工有限公司 | A kind of high-content Bravo continuous rectification purifying technique |
| CN109289739A (en) * | 2018-10-29 | 2019-02-01 | 江苏维尤纳特精细化工有限公司 | A kind of Bravo production logical chlorine automatic control device and its method |
| CN109293529A (en) * | 2018-12-06 | 2019-02-01 | 江苏新河农用化工有限公司 | A kind of purifying plant and method producing Bravo of the hexachloro-benzene no more than 10ppm |
| CN109369454A (en) * | 2018-12-06 | 2019-02-22 | 江苏新河农用化工有限公司 | A kind of unqualified Bravo continuous rectification purification system and method |
| CN109438284A (en) * | 2018-12-06 | 2019-03-08 | 江苏新河农用化工有限公司 | A kind of continuous rectification purifying technique of low content Bravo |
| CN109760162A (en) * | 2019-01-24 | 2019-05-17 | 深圳市至霸化工有限公司 | A kind of bamboo and wood rattan willow herb mildew and insect proof fungicide |
| 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 |
| CN111285783A (en) * | 2018-12-06 | 2020-06-16 | 上海泰禾国际贸易有限公司 | Refining and purifying system and method for high-content chlorothalonil |
| CN111285784A (en) * | 2018-12-06 | 2020-06-16 | 上海泰禾国际贸易有限公司 | Unqualified chlorothalonil purification system and method |
| CN111870988A (en) * | 2020-07-17 | 2020-11-03 | 江苏新河农用化工有限公司 | Trapping method and trapping system for tetrachloroisophthalonitrile reaction gas |
| CN112939812A (en) * | 2021-02-07 | 2021-06-11 | 江苏新河农用化工有限公司 | Chlorothalonil production process |
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| DE1158500B (en) * | 1962-04-06 | 1963-12-05 | Bayer Ag | Process for the production of polyisonitriles |
| US3839401A (en) * | 1972-10-17 | 1974-10-01 | Diamond Shamrock Corp | Fluid bed chlorination of phthalonitriles |
| US4485050A (en) * | 1982-05-13 | 1984-11-27 | Caffaro S.P.A. | Process for the continuous production of tetrachlorophthalonitrile in a fluidized bed reactor |
| CN1948278A (en) * | 2006-11-07 | 2007-04-18 | 云南省化工研究院 | Production method of low hexachlorobenzene content chlorothalonil |
| CN102718682A (en) * | 2011-03-29 | 2012-10-10 | 张苏侠 | Preparation method for chlorothalonil |
| CN104447407A (en) * | 2014-12-08 | 2015-03-25 | 江阴苏利化学股份有限公司 | Method of preparing chlorothalonil with hexachlorobenzene content lower than 10ppm |
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- 2016-10-20 CN CN201610915081.7A patent/CN107056650A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| DE1158500B (en) * | 1962-04-06 | 1963-12-05 | Bayer Ag | Process for the production of polyisonitriles |
| US3839401A (en) * | 1972-10-17 | 1974-10-01 | Diamond Shamrock Corp | Fluid bed chlorination of phthalonitriles |
| US4485050A (en) * | 1982-05-13 | 1984-11-27 | Caffaro S.P.A. | Process for the continuous production of tetrachlorophthalonitrile in a fluidized bed reactor |
| CN1948278A (en) * | 2006-11-07 | 2007-04-18 | 云南省化工研究院 | Production method of low hexachlorobenzene content chlorothalonil |
| CN102718682A (en) * | 2011-03-29 | 2012-10-10 | 张苏侠 | Preparation method for chlorothalonil |
| CN104447407A (en) * | 2014-12-08 | 2015-03-25 | 江阴苏利化学股份有限公司 | Method of preparing chlorothalonil with hexachlorobenzene content lower than 10ppm |
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108329235B (en) * | 2018-03-02 | 2020-10-02 | 天津赛普泰克科技有限公司 | Process for producing high-purity chlorothalonil |
| CN109289739A (en) * | 2018-10-29 | 2019-02-01 | 江苏维尤纳特精细化工有限公司 | A kind of Bravo production logical chlorine automatic control device and its method |
| CN111285783A (en) * | 2018-12-06 | 2020-06-16 | 上海泰禾国际贸易有限公司 | Refining and purifying system and method for high-content chlorothalonil |
| CN109438284B (en) * | 2018-12-06 | 2021-12-07 | 江苏新河农用化工有限公司 | Continuous rectification purification process for low-content chlorothalonil |
| CN109438284A (en) * | 2018-12-06 | 2019-03-08 | 江苏新河农用化工有限公司 | A kind of continuous rectification purifying technique of low content Bravo |
| CN109293529B (en) * | 2018-12-06 | 2023-11-24 | 江苏新河农用化工有限公司 | Purifying device and method for producing chlorothalonil with content of hexachlorobenzene not more than 10ppm |
| CN109369454B (en) * | 2018-12-06 | 2023-11-24 | 江苏新河农用化工有限公司 | Continuous rectification and purification system and method for unqualified chlorothalonil |
| CN109293529A (en) * | 2018-12-06 | 2019-02-01 | 江苏新河农用化工有限公司 | A kind of purifying plant and method producing Bravo of the hexachloro-benzene no more than 10ppm |
| CN111285784A (en) * | 2018-12-06 | 2020-06-16 | 上海泰禾国际贸易有限公司 | Unqualified chlorothalonil purification system and method |
| CN109265365A (en) * | 2018-12-06 | 2019-01-25 | 江苏新河农用化工有限公司 | A kind of high-content Bravo continuous rectification purifying technique |
| CN111285784B (en) * | 2018-12-06 | 2023-04-18 | 江苏新河农用化工有限公司 | Unqualified chlorothalonil purification system and method |
| CN111285783B (en) * | 2018-12-06 | 2023-04-18 | 江苏新河农用化工有限公司 | Refining and purifying system and method for high-content chlorothalonil |
| CN109369454A (en) * | 2018-12-06 | 2019-02-22 | 江苏新河农用化工有限公司 | A kind of unqualified Bravo continuous rectification purification system and method |
| CN109760162A (en) * | 2019-01-24 | 2019-05-17 | 深圳市至霸化工有限公司 | A kind of bamboo and wood rattan willow herb mildew and insect proof fungicide |
| CN110845366B (en) * | 2019-12-03 | 2022-09-20 | 万华化学集团股份有限公司 | Preparation method and preparation system of chlorothalonil |
| 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 |
| CN111870988A (en) * | 2020-07-17 | 2020-11-03 | 江苏新河农用化工有限公司 | Trapping method and trapping system for tetrachloroisophthalonitrile reaction gas |
| CN112939812A (en) * | 2021-02-07 | 2021-06-11 | 江苏新河农用化工有限公司 | Chlorothalonil production process |
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Application publication date: 20170818 |
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