CN102603664B - Method and device for producing clomazone - Google Patents
Method and device for producing clomazone Download PDFInfo
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- CN102603664B CN102603664B CN201210034961.5A CN201210034961A CN102603664B CN 102603664 B CN102603664 B CN 102603664B CN 201210034961 A CN201210034961 A CN 201210034961A CN 102603664 B CN102603664 B CN 102603664B
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Abstract
The invention belongs to the field of pesticide production, and particularly discloses a method and a device for producing clomazone. A tubular reactor is designed into two sections, and the internal temperatures of the two pipe sections are respectively controlled in a production process, so that reactants in the tubular reactor are respectively kept in different temperature ranges; and a catalyst is added into the tubular reactor to shorten the reaction time of a product and avoid producing impurities caused by long-time contact. The method and the device provided by the invention make use of the particularity of temperature controllability of the tubular reactor in the production process and the reaction contact time decreased by the catalyst to increase the product yield and shorten the reaction period.
Description
(1) technical field
The invention belongs to field of pesticide production, particularly a kind of method and apparatus producing clomazone.
(2) background technology
Clomazone is the organic heterocyclic class selectivity herbicide before seedling stage of Fu Meishi company of the U.S. (FMC Corporation) Development and Production, is applicable to prevent and kill off soybean, the annual gramineous weed of fields of peanut and other crops and broadleaf weeds.By root, the young shoot absorption of plant, upwards dredge, diffuse to leaf portion through xylem, suppress the chlorophyll of sensitive plant and the synthesis of carotene, form white seedling, dead in a short time, sustainable more than 6 months of the biological activity of lasting period long ， clomazone in soil, can under recommended dose, selectivity arranges succession crop, avoids key.
By Chinese pesticide toxicity grading criteria, clomazone belongs to low toxicity herbicide, and primary synthetic methods has the synthetic method such as o-chlorobenzaldehyde method, Chloropivaloyl chloride method, the operational path that many manufacturing enterprises of Chloropivaloyl chloride Fa Shi China generally adopt.China's clomazone synthesis generally adopts autoclave Autoclave, and its single covering device ability is little, and in reactant still, the residence time is long, energy consumption is high, level of automation is low, unstable product quality, is unfavorable for the stably manufactured of clomazone.
(3) summary of the invention
The present invention, in order to make up the deficiencies in the prior art, provides the method and apparatus that a kind of product generates the production clomazone stable, level of automation is high.
The present invention is achieved through the following technical solutions:
Produce a method for clomazone, mainly comprise the steps:
(1) raw material oxammonium hydrochloride liquid, Chloropivaloyl chloride and adjacent chlorobenzyl chloride are fully mixed respectively by fresh feed pump feeding mixing tank;
(2) sent into by mixed liquor in low temperature tubular reactor, in low temperature tubular reactor, pass into liquid caustic soda simultaneously promote reaction, low temperature tubular type temperature of reactor controls at 0 ~ 30 DEG C;
(3) reaction material of preventing and kill off from low temperature tubular reactor is by sending into high-temperature tubular reactor after preheater heating, and in high-temperature tubular reactor, pass into catalyzer, in high-temperature tubular reactor, temperature controls at 80 ~ 85 DEG C simultaneously;
(4) send into quantizer from the reaction product of high-temperature tubular reactor release, water layer sends into wastewater treatment pipe, and product is collected after thin film evaporation.
Tubular reactor is set to two sections by the present invention, respectively two segment pipe internal temperatures are controlled when producing, thus make reactant be in different temperature ranges respectively in tubular reactor, catalyzer is added in tubular reactor, the product reaction times is shortened, avoids Long contact time and produce impurity.
More excellent scheme of the present invention is:
Described catalyzer is crown ether compound, quaternary ammonium salt, tertiary amine inorganic acid salt or strong alkaline tertiary amine.
The reaction times of described material in low temperature tubular reactor is the half in reaction times in high-temperature tubular reactor.
Described catalyzer is the crown compound containing 4 ~ 6 oxygen, as 12-crown ether-4,15-crown ether-5, hexaoxacyclooctadecane-6-6,30-crown ether-10.
The device of production clomazone of the present invention, comprise the large tank of oxammonium hydrochloride liquid, the large tank of Chloropivaloyl chloride and the large tank of adjacent chlorobenzyl chloride, it is characterized in that: described three large tanks are communicated with mixing tank respectively by fresh feed pump, mixing tank is communicated with low temperature tubular reactor, the large tank of liquid caustic soda is communicated with by the feed-pipe of fresh feed pump with low temperature tubular reactor, low temperature tubular reactor is connected with high-temperature tubular reactor by preheater, and the discharge port of high-temperature tubular reactor is connected with quantizer.
Described delaminator tip outlet is provided with wastewater treatment pipe, bottom end outlet is provided with thin film evaporation pipe, water layer, directly through sewage works process, stores after product-collecting or takes out.
Be provided with chilled brine cooling pipe in described low temperature tubular reactor, in high-temperature tubular reactor, be provided with steam heating tube.
The charging line of each large tank of described connection is provided with under meter.
The duct length of described low temperature tubular reactor is less than the duct length of high-temperature tubular reactor.
The reaction contact time that when the present invention utilizes tubular reactor produced, the singularity of temperature control and catalyzer reduce, the product yield obtained is improved, and reaction time reduces, and uses this device simple to operate, level of automation is high, effectively can reduce labour intensity.
(4) accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further illustrated.
Fig. 1 is apparatus structure schematic diagram of the present invention.
In figure, the large tank of 1 oxammonium hydrochloride liquid, 2 fresh feed pumps, 3 under meters, the large tank of 4 Chloropivaloyl chloride, the large tank of 5 adjacent chlorobenzyl chloride, the large tank of 6 liquid caustic soda, the large tank of 7 catalyzer, 8 mixing tanks, 9 low temperature tubular reactors, 10 preheaters, 11 high-temperature tubular reactors, 12 quantizers, 13 wastewater treatment pipes, 14 thin film evaporation pipes.
(5) embodiment
Accompanying drawing is a kind of specific embodiment of the present invention.This embodiment comprises the large tank of oxammonium hydrochloride liquid 1, the large tank of Chloropivaloyl chloride 4 and the large tank 5 of adjacent chlorobenzyl chloride, described three large tanks are communicated with mixing tank 8 respectively by fresh feed pump 2, mixing tank 8 is communicated with low temperature tubular reactor 9, the large tank 6 of liquid caustic soda is communicated with the feed-pipe of low temperature tubular reactor 9 by fresh feed pump 2, low temperature tubular reactor 9 is connected with high-temperature tubular reactor 11 by preheater 10, the discharge port of high-temperature tubular reactor 11 is connected with quantizer 12; The outlet of described quantizer 12 top is provided with wastewater treatment pipe 13, bottom end outlet is provided with thin film evaporation pipe 14; Be provided with chilled brine cooling pipe in described low temperature tubular reactor 9, in high-temperature tubular reactor 11, be provided with steam heating tube; The charging line of each large tank of described connection is provided with under meter 3; The duct length of low temperature tubular reactor 9 is less than the duct length of high-temperature tubular reactor 11.
First by the raw material 25% hydrochloric acid hydroxyl liquid of He Cheng clomazone, squeeze into the large tank of oxammonium hydrochloride liquid 1, Chloropivaloyl chloride squeezes into the large tank 4 of Chloropivaloyl chloride, adjacent chlorobenzyl chloride squeezes into the large tank 5 of adjacent chlorobenzyl chloride, then mixing in mixing tank 8 is flowed into the flow velocity of 2:1:1, send in low temperature tubular reactor 9, liquid caustic soda enters in mixture with the flow velocity of Chloropivaloyl chloride 3 times and promotes reaction simultaneously.
Reactant flow the first step reaction when through low temperature tubular reactor 9 end terminates, reactant is preheated to 80 DEG C through preheater 10 and enters high-temperature tubular reactor 11, catalyzer crown ether enters pipeline promotion reaction with Chloropivaloyl chloride 0.05 times of flow velocity simultaneously, reactant completes through high-temperature tubular reactor 11 end reaction, then feed liquid enters quantizer 12 and carries out layered shaping, upper strata waste water carries out wastewater treatment, and lower floor's feed liquid obtains the finished product through thin film evaporation.
Claims (8)
1. produce a method for clomazone, it is characterized by, mainly comprise the steps:
(1) raw material oxammonium hydrochloride liquid, Chloropivaloyl chloride and adjacent chlorobenzyl chloride are fully mixed respectively by fresh feed pump feeding mixing tank;
(2) sent into by mixed liquor in low temperature tubular reactor, in low temperature tubular reactor, pass into liquid caustic soda simultaneously promote reaction, low temperature tubular type temperature of reactor controls at 0 ~ 30 DEG C;
(3) reaction material of releasing from low temperature tubular reactor is by sending into high-temperature tubular reactor after preheater heating, and in high-temperature tubular reactor, pass into catalyzer, in high-temperature tubular reactor, temperature controls at 80 ~ 85 DEG C simultaneously; Described catalyzer is crown ether compound, quaternary ammonium salt, tertiary amine inorganic acid salt or strong alkaline tertiary amine;
(4) send into quantizer from the reaction product of high-temperature tubular reactor release, water layer sends into wastewater treatment pipe, and product is collected after thin film evaporation.
2. the method for production clomazone according to claim 1, is characterized in that: the reaction times of described mixed liquor in low temperature tubular reactor is the half in reaction times in high-temperature tubular reactor.
3. the method for production clomazone according to claim 2, is characterized in that: described catalyzer is the crown compound containing 4 ~ 6 oxygen.
4. the device of production clomazone according to claim 1, comprise the large tank of oxammonium hydrochloride liquid (1), the large tank of Chloropivaloyl chloride (4) and the large tank of adjacent chlorobenzyl chloride (4), it is characterized in that: described three large tanks are communicated with mixing tank (8) respectively by fresh feed pump (2), mixing tank (8) is communicated with low temperature tubular reactor (9), the large tank of liquid caustic soda (6) is communicated with by the feed-pipe of fresh feed pump (2) with low temperature tubular reactor (9), low temperature tubular reactor (9) is connected with high-temperature tubular reactor (11) by preheater (10), the discharge port of high-temperature tubular reactor (11) is connected with quantizer (12).
5. the device of production clomazone according to claim 4, is characterized in that: the outlet of described quantizer (12) top is provided with wastewater treatment pipe (13), bottom end outlet is provided with thin film evaporation pipe (14).
6. the device of production clomazone according to claim 4, is characterized in that: be provided with chilled brine cooling pipe in described low temperature tubular reactor (9), high-temperature tubular reactor is provided with steam heating tube in (11).
7. the device of production clomazone according to claim 4, is characterized in that: the charging line of each large tank of described connection is provided with under meter (3).
8. the device of production clomazone according to claim 4, is characterized in that: the duct length of described low temperature tubular reactor (9) is less than the duct length of high-temperature tubular reactor (11).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210034961.5A CN102603664B (en) | 2012-02-16 | 2012-02-16 | Method and device for producing clomazone |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210034961.5A CN102603664B (en) | 2012-02-16 | 2012-02-16 | Method and device for producing clomazone |
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| CN102603664A CN102603664A (en) | 2012-07-25 |
| CN102603664B true CN102603664B (en) | 2014-12-24 |
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| CN201210034961.5A Active CN102603664B (en) | 2012-02-16 | 2012-02-16 | Method and device for producing clomazone |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11649219B2 (en) | 2013-07-03 | 2023-05-16 | Rotam Agrochem International Company Limited | Process for preparing a clomazone, novel form and use of the same |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202658106U (en) * | 2012-02-16 | 2013-01-09 | 潍坊先达化工有限公司 | Clomazone production device |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202658106U (en) * | 2012-02-16 | 2013-01-09 | 潍坊先达化工有限公司 | Clomazone production device |
Non-Patent Citations (1)
| Title |
|---|
| 何怡锐.2-(2-氯苯基)甲基-4,4-二甲基-3-异噁唑酮合成方法的研究.《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》.2008,B016-53. * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11649219B2 (en) | 2013-07-03 | 2023-05-16 | Rotam Agrochem International Company Limited | Process for preparing a clomazone, novel form and use of the same |
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| CN102603664A (en) | 2012-07-25 |
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Effective date of registration: 20211130 Address after: 261000 East 2nd house, Lingang chemical park, Binhai Economic Development Zone, Weifang City, Shandong Province Patentee after: WEIFANG CYNDA CHEMICAL Co.,Ltd. Patentee after: Shandong Xianda agrochemical Co., Ltd Address before: 261000 Lingang Chemical Park, Weifang Binhai Economic Development Zone, Shandong Province Patentee before: WEIFANG CYNDA CHEMICAL Co.,Ltd. |
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