CN204369783U - A kind of continuous process system of Azoxystrobin - Google Patents
A kind of continuous process system of Azoxystrobin Download PDFInfo
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- CN204369783U CN204369783U CN201520006039.4U CN201520006039U CN204369783U CN 204369783 U CN204369783 U CN 204369783U CN 201520006039 U CN201520006039 U CN 201520006039U CN 204369783 U CN204369783 U CN 204369783U
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- tank
- strainer
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- pipeline
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- CUEDLSLTSIRGCF-CLFYSBASSA-N CO/C=C(\C(OC)=O)/c1ccccc1O Chemical compound CO/C=C(\C(OC)=O)/c1ccccc1O CUEDLSLTSIRGCF-CLFYSBASSA-N 0.000 description 2
- YRYZZSRRDCTETP-FLIBITNWSA-N CO/C=C(\C(OC)=O)/c1ccccc1Oc1cc(Cl)ncn1 Chemical compound CO/C=C(\C(OC)=O)/c1ccccc1Oc1cc(Cl)ncn1 YRYZZSRRDCTETP-FLIBITNWSA-N 0.000 description 2
- XJPZKYIHCLDXST-UHFFFAOYSA-N Clc1ncnc(Cl)c1 Chemical compound Clc1ncnc(Cl)c1 XJPZKYIHCLDXST-UHFFFAOYSA-N 0.000 description 2
- CHZCERSEMVWNHL-UHFFFAOYSA-N N#Cc(cccc1)c1O Chemical compound N#Cc(cccc1)c1O CHZCERSEMVWNHL-UHFFFAOYSA-N 0.000 description 2
- JNEZGHPSXFUFMT-UHFFFAOYSA-N N#Cc(cccc1)c1Oc1cc(Cl)ncn1 Chemical compound N#Cc(cccc1)c1Oc1cc(Cl)ncn1 JNEZGHPSXFUFMT-UHFFFAOYSA-N 0.000 description 2
- WFDXOXNFNRHQEC-LGMDPLHJSA-N CO/C=C(\C(OC)=O)/c1ccccc1Oc1ncnc(Oc(cccc2)c2C#N)c1 Chemical compound CO/C=C(\C(OC)=O)/c1ccccc1Oc1ncnc(Oc(cccc2)c2C#N)c1 WFDXOXNFNRHQEC-LGMDPLHJSA-N 0.000 description 1
- CMFNCDDGGKUFFW-UHFFFAOYSA-N COCC(C(OC)=O)c1ccccc1Oc1ncnc(Oc(cccc2)c2C#N)c1 Chemical compound COCC(C(OC)=O)c1ccccc1Oc1ncnc(Oc(cccc2)c2C#N)c1 CMFNCDDGGKUFFW-UHFFFAOYSA-N 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model relates to a kind of continuous process system of Azoxystrobin, comprise the feed system, reactive system and the separation and purification system that connect successively, described feed system comprises 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate head tank, the chloro-6-of 4-(2-cyano-benzene oxygen) pyrimidine starting material tank, N, dinethylformamide head tank and two batching kettles, described reactive system comprises the mixing tank, reactor and the thick products pot that connect successively, and described separation and purification system comprises the first strainer, crystallization kettle, the second strainer and the moisture eliminator that connect successively.Native system adopts continuous tubular reactor to replace traditional tank reactor, ceramic packing is provided with in reactor tube, enhance heat transfer and the mass transfer of reaction, make reaction rate accelerates, avoid 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate be heated for a long time and side reaction occurs, make reaction yield reach more than 90%, production efficiency significantly improves.
Description
Technical field
The utility model belongs to chemical field, relates to the production of Azoxystrobin, especially a kind of continuous process system of Azoxystrobin.
Background technology
Azoxystrobin is a kind of methoxy acrylic bactericide, possess the features such as efficient, wide spectrum, low toxicity, good activity is all had to nearly all Eumycetes disease such as Powdery Mildew, rust, glume blight, net blotch, oidium, rice blast etc., can be used for cauline leaf spraying, seed treatment, soil treatment, be mainly used in cereal, paddy rice, peanut, grape, potato, fruit tree, vegetables etc.
Patent WO2008043978A1 discloses the synthetic route of following two kinds of Azoxystrobin.All use intermediate 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate (3) as intermediate in two kinds of synthetic routes, this intermediate is unstable, when the long period is heated, hydrolysis reaction in molecule can occur, the reaction yield causing this intermediate to participate in is lower.
Patent CN102311392A discloses a kind of method of improvement, shown in use formula (5), compound first synthesizes 2-[2-(6-chloropyrimide-4 base oxygen base) phenyl]-3 as intermediate, 3-dimethoxy methyl propionate, then demethoxylation obtains intermediate (4), and reaction process is as follows:
Shown in formula (4), compound is unstable, when heated time is longer, equally hydrolysis reaction in molecule can occur, reaction yield is reduced.
Described in patent WO2008043978A1 and CN102311392A, reaction process all adopts tank reactor, periodical operation, reaction mass adds simultaneously, this reaction belongs to thermopositive reaction, due to the heat transfer of tank reactor and mass-transfer efficiency lower, cause speed of reaction slower, reaction heat is not easy remove and cause temperature to raise, make formula (3) and formula (5) described unstable compound residence time in reactor longer, temperature is too high, causes yield lower.
Utility model content
Technical problem to be solved in the utility model is for route described in reaction formula 1, provide a kind of heat transfer and mass transfer effect good, effectively can increase each reaction mass contact area, the continuous process system of the Azoxystrobin of Reaction time shorten.
The technical scheme that the utility model technical solution problem adopts is:
A kind of continuous process system of Azoxystrobin, comprise the feed system connected successively, reactive system and separation and purification system, described feed system comprises 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate head tank, the chloro-6-of 4-(2-cyano-benzene oxygen) pyrimidine starting material tank, N, dinethylformamide head tank and two batching kettles, described reactive system comprises the mixing tank connected successively, reactor and thick products pot, described separation and purification system comprises the first strainer connected successively, crystallization kettle, second strainer and moisture eliminator, 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate head tank, the chloro-6-of 4-(2-cyano-benzene oxygen) pyrimidine starting material tank and N, dinethylformamide head tank pipeline connects batching kettle, described batching kettle pipeline connects mixing tank, mixing tank pipeline ligation device top opening for feed, described reactor is tubular reactor, reactor lower end discharge opening pipeline connects thick product storage tank upper end opening for feed, thick product storage tank lower end discharge opening pipeline connects the first strainer, first strainer lower end liquid outlet opening pipeline connects crystallization kettle upper end opening for feed, crystallization kettle lower end discharge opening pipeline connects the second strainer, second strainer lower end solids exit mouth pipeline connects moisture eliminator, crystallization kettle upper end pipeline connects methanol tank, crystallization kettle is provided with condenser and DMF discharge port.
And 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate mixes in the first batching kettle with DMF; The chloro-6-of 4-(2-cyano-benzene oxygen) pyrimidine mixes in the second batching kettle with DMF.
And, the pipeline that 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate head tank, the chloro-6-of 4-(2-cyano-benzene oxygen) pyrimidine storage tank head tank and DMF head tank are connected with batching kettle is equipped with volume pump.
And, the pipeline that described batching kettle is connected with mixing tank is equipped with volume pump.
And described reactor is temperature control, shell and tube reactor, in pipe, be provided with ceramic ring filler or structured ceramic packing.
And, be equipped with volume pump at the first strainer with on the pipeline be connected with the second strainer on the pipeline be connected with crystallization kettle on the tank connected pipeline of thick product, at the first strainer, at crystallization kettle.
And described crystallization kettle is batch still, be provided with stirring rake, condenser and heating jacket.
And described strainer is pressure filter or drum filter or liquid filter.
And described moisture eliminator is continuously feeding moisture eliminator.
And described continuously feeding moisture eliminator is vacuum box type moisture eliminator or tunnel drier or channel oven.
Advantage of the present utility model and positively effect are:
1, native system by two intermediate 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate and the chloro-6-of 4-(2-cyano-benzene oxygen) pyrimidine respectively with solvent N, after dinethylformamide first mixes in batching kettle, continue through mixing tank according to a certain percentage again, in mixing tank, two intermediates meet, mix, then enter into reactor fast to react, it is very even that the design of this feed system makes the material entered in reactor be mixed to get, and the reactant reaction speed mixed is fast, react completely, by product is few, yield is high.
2, native system adopts continuous tubular reactor to replace traditional tank reactor, ceramic ring filler or structured ceramic packing is provided with in reactor tube, reactant can be made in pipe in turbulent flows, add reactant contact area, reduce resistance to flow, less to the solid product resistance in reaction system, avoid solid materials to be trapped.
The heat transfer of the filler-reinforced reaction 3, be provided with in native system reactor tube and mass transfer, reaction rate accelerates can be made, and keep constant temperature of reaction, make 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate intermediate shorter residence time in reactor, avoid it to be heated for a long time and the hydrolytic side reactions occurred, make reaction yield reach more than 90%, achieve continuous prodution, production efficiency significantly improves.
Accompanying drawing explanation
Fig. 1 is the structural representation of native system.
Embodiment
Below in conjunction with accompanying drawing, also by specific embodiment, the utility model is described in further detail, and following examples are descriptive, are not determinate, can not limit protection domain of the present utility model with this.
A continuous process system for Azoxystrobin, comprises the feed system, reactive system and the separation and purification system that connect successively.
Described feed system comprises 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate head tank 1, the chloro-6-of 4-(2-cyano-benzene oxygen) pyrimidine starting material tank 14, N, dinethylformamide head tank 15 and two batching kettles, wherein 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate head tank is connected with the top opening for feed pipeline of the first batching kettle 3 by volume pump 2, the chloro-6-of 4-(2-cyano-benzene oxygen) pyrimidine starting material tank is connected with the top opening for feed pipeline of the second batching kettle 13 by volume pump, N, dinethylformamide head tank is connected with the top opening for feed pipeline of the first batching kettle and the second batching kettle respectively by volume pump.
Described reactive system comprises the mixing tank 4 connected successively, reactor 5 and thick products pot 12, the top opening for feed of described mixing tank is connected with the discharge port of the first batching kettle and the discharge opening pipeline of the second batching kettle respectively by volume pump, described reactor is shell and tube reactor, water is adopted to carry out heating and cooling, reactant walks tube side, water walks shell side, ceramic ring filler or structured ceramic packing is provided with in pipe, reactant can be made in pipe in turbulent flows, increase reactant contact area, reduce resistance to flow, less to the solid product resistance in reaction system, solid materials is avoided to be trapped, be preferably structured ceramic packing.And, be provided with temperature-control device in reactor, controlled the temperature of reactor by temperature-control device.
Described separation and purification system comprises the first strainer 11, crystallization kettle 10, second strainer 9 and the moisture eliminator 8 that connect successively, the opening for feed of described first strainer is connected by the discharge opening pipeline of volume pump with thick products pot, the liquid outlet opening of this first strainer is connected with the opening for feed pipeline of crystallization kettle by volume pump, the bottom discharge port of this crystallization kettle is connected with the opening for feed pipeline of the second strainer by volume pump, and the solids exit mouth of this second strainer is connected with the opening for feed pipeline of moisture eliminator.Stirring rake is provided with in crystallization kettle, heating jacket is provided with at the outer wall of crystallization kettle, a condenser 6 is connected at the top discharge port of crystallization kettle, liquid in crystallization kettle is heated by the water vapour in heating jacket, make solvent DMF (N, dinethylformamide) steam, DMF enters into condenser, enters into DMF withdrawing can after condensation.A methanol tank 7 is also connected with by volume pump at the top opening for feed of crystallization kettle, for methyl alcohol is pumped in crystallization kettle, the solid product that dissolving crystallized still intercrystalline goes out.
Principle of work of the present utility model is:
By intermediate 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate, solvent DMF (DMF), K
2cO
3and DABCO joins the first batching kettle (being labeled as mixture 1), chloro-for intermediate 4-6-(2-cyano-benzene oxygen) pyrimidine and solvent DMF are joined the second batching kettle (being labeled as mixture 2), by volume pump, mixture 1 and mixture 2 are continued through mixing tank according to a certain percentage after mixing respectively, then mixture enters into the reactor with temperature control unit, pass through reactor from top to down, keep constant temperature in reactor, control mixture flow by volume pump and control the reaction times, the thick product generated is deposited in thick product storage tank, this thick product storage tank is furnished with emptying device and keeps normal pressure, then thick product is pumped in the first strainer by volume pump and filters, liquid enters crystallization kettle, the solid materials filtered out is discharged from strainer, enter the liquid of crystallization kettle, by the water vapour heating in heating jacket, DMF is steamed and enters into condenser, DMF withdrawing can is entered into after condensation, methyl alcohol is entered in crystallization kettle by volume pump, heating for dissolving solid, be cooled to room temperature, crystal is separated out, solid-liquid mixture is pumped into the second strainer inner filtration by volume pump, liquid enters into Methanol Recovery tank, in second strainer, solid by filtration device lower end valve enters in moisture eliminator, obtain Azoxystrobin product after drying.
Embody rule embodiment:
As shown in Figure 1, in reactor, be provided with tubulation 100, every root diameter 100mm, pipe range 2000mm, pipe built with ceramic filler, by 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate 416kg, DMF1m
3(944kg), K
2cO
3414kg and DABCO5.824kg joins in first batching kettle of 2 cubic metres and stirs, and then joins mixing tank with the flow of 17.8kg/h, by chloro-for 4-6-(2-cyano-benzene oxygen) pyrimidine 462kg, DMF1m
3(944kg) join in second batching kettle of 2 cubic metres and stir, then join mixing tank with the flow of 14.06kg/h, in mixing tank, material joins in reactor with the flow of 31.86kg/h, and after 2min, outflow reactor enters thick products pot.Thick product once pumps into 765kg from thick products pot through volume pump to strainer, and filtered fluid 763kg enters into crystallization kettle, removes DMF, pump into methyl alcohol 0.3m by volume pump in crystallization kettle by the distillation of jacket water (J.W.) steam-heated cal(l)andria
3, be heated to 50 DEG C, dissolution of solid, be pumped in strainer filter after cooling by volume pump, solid 192kg to be transported in moisture eliminator after dry 10h, obtains Azoxystrobin 174kg, yield 90%.
Above-described is only preferred implementation of the present utility model; it should be pointed out that for the person of ordinary skill of the art, under the prerequisite not departing from utility model design; can also make some distortion and improvement, these all belong to protection domain of the present utility model.
Claims (10)
1. the continuous process system of an Azoxystrobin, it is characterized in that: comprise the feed system connected successively, reactive system and separation and purification system, described feed system comprises 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate head tank, the chloro-6-of 4-(2-cyano-benzene oxygen) pyrimidine starting material tank, N, dinethylformamide head tank and two batching kettles, described reactive system comprises the mixing tank connected successively, reactor and thick products pot, described separation and purification system comprises the first strainer connected successively, crystallization kettle, second strainer and moisture eliminator, 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate head tank, the chloro-6-of 4-(2-cyano-benzene oxygen) pyrimidine starting material tank and N, dinethylformamide head tank pipeline connects batching kettle, described batching kettle pipeline connects mixing tank, mixing tank pipeline ligation device top opening for feed, described reactor is tubular reactor, reactor lower end discharge opening pipeline connects thick product storage tank upper end opening for feed, thick product storage tank lower end discharge opening pipeline connects the first strainer, first strainer lower end liquid outlet opening pipeline connects crystallization kettle upper end opening for feed, crystallization kettle lower end discharge opening pipeline connects the second strainer, second strainer lower end solids exit mouth pipeline connects moisture eliminator, crystallization kettle upper end pipeline connects methanol tank, crystallization kettle is provided with condenser and DMF discharge port.
2. the continuous process system of Azoxystrobin according to claim 1, is characterized in that: 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate mixes in the first batching kettle with DMF; The chloro-6-of 4-(2-cyano-benzene oxygen) pyrimidine mixes in the second batching kettle with DMF.
3. the continuous process system of Azoxystrobin according to claim 1, it is characterized in that: on the pipeline that 2-(2-hydroxy phenyl)-3-methoxy-methyl acrylate head tank, the chloro-6-of 4-(2-cyano-benzene oxygen) pyrimidine storage tank head tank and DMF head tank are connected with batching kettle, be equipped with volume pump.
4. the continuous process system of Azoxystrobin according to claim 1, is characterized in that: on the pipeline that described batching kettle is connected with mixing tank, be equipped with volume pump.
5. the continuous process system of Azoxystrobin according to claim 1, is characterized in that: described reactor is temperature control, shell and tube reactor, is provided with ceramic ring filler or structured ceramic packing in pipe.
6. the continuous process system of Azoxystrobin according to claim 1, is characterized in that: be equipped with volume pump at the first strainer with on the pipeline be connected with the second strainer on the pipeline be connected with crystallization kettle on the tank connected pipeline of thick product, at the first strainer, at crystallization kettle.
7. the continuous process system of Azoxystrobin according to claim 1, is characterized in that: described crystallization kettle is batch still, is provided with stirring rake, condenser and heating jacket.
8. the continuous process system of Azoxystrobin according to claim 1, is characterized in that: described strainer is pressure filter or drum filter or liquid filter.
9. the continuous process system of Azoxystrobin according to claim 1, is characterized in that: described moisture eliminator is continuously feeding moisture eliminator.
10. the continuous process system of Azoxystrobin according to claim 9, is characterized in that: described continuously feeding moisture eliminator is vacuum box type moisture eliminator or tunnel drier or channel oven.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201520006039.4U CN204369783U (en) | 2015-01-05 | 2015-01-05 | A kind of continuous process system of Azoxystrobin |
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| CN201520006039.4U CN204369783U (en) | 2015-01-05 | 2015-01-05 | A kind of continuous process system of Azoxystrobin |
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| CN204369783U true CN204369783U (en) | 2015-06-03 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107118163A (en) * | 2017-05-12 | 2017-09-01 | 上海开荣化工科技有限公司 | Fluoxastrobin production line |
| CN111533914A (en) * | 2020-04-13 | 2020-08-14 | 浙江衢州正邦有机硅有限公司 | Continuous production process of polymethyltriethoxysilane in pipeline mode |
-
2015
- 2015-01-05 CN CN201520006039.4U patent/CN204369783U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107118163A (en) * | 2017-05-12 | 2017-09-01 | 上海开荣化工科技有限公司 | Fluoxastrobin production line |
| CN111533914A (en) * | 2020-04-13 | 2020-08-14 | 浙江衢州正邦有机硅有限公司 | Continuous production process of polymethyltriethoxysilane in pipeline mode |
| CN111533914B (en) * | 2020-04-13 | 2022-08-02 | 郑启波 | Continuous production process of polymethyltriethoxysilane in pipeline mode |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150603 Termination date: 20200105 |
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| CF01 | Termination of patent right due to non-payment of annual fee |