CN108499508B - A kind of multipoles reactors and the method for preparing cycocel using the device - Google Patents
A kind of multipoles reactors and the method for preparing cycocel using the device Download PDFInfo
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- CN108499508B CN108499508B CN201810562564.2A CN201810562564A CN108499508B CN 108499508 B CN108499508 B CN 108499508B CN 201810562564 A CN201810562564 A CN 201810562564A CN 108499508 B CN108499508 B CN 108499508B
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- reaction kettle
- cycocel
- head tank
- order reaction
- multipoles
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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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1862—Stationary reactors having moving elements inside placed in series
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/80—Mixing plants; Combinations of mixers
- B01F33/82—Combinations of dissimilar mixers
- B01F33/821—Combinations of dissimilar mixers with consecutive receptacles
-
- 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
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/04—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups
- C07C209/06—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms
- C07C209/12—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms with formation of quaternary ammonium compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of multipoles reactors, including the head tank one being sequentially connected in series, mixing vessel and n order reaction kettle.The multipoles reactors further include head tank two, and the head tank one and head tank two are arranged in parallel；Wherein n is the integer of 3-10；Pressure reducing valve is provided between the (n-1)th order reaction kettle and the n-th order reaction kettle.The invention also discloses a kind of methods for preparing cycocel using multipoles reactors, comprising the following steps: dichloroethanes is added in head tank one, trimethylamine is added in head tank two；Above two raw material is passed through in static mixer and is sufficiently mixed；By in mixer dichloroethanes and trimethylamine be successively passed through n-1 order reaction kettle；After pressure reducing valve depressurizes, into the n-th order reaction kettle.Cycocel will can be obtained after centrifugation drying by n order reaction kettle feed liquid, the dichloroethanes mother liquor after centrifugation is passed through head tank one and is recycled.The present invention has the characteristics of fully reacting, low cost, high benefit.
Description
Technical field
The invention belongs to compound synthesis field, in particular to a kind of multipoles reactors and using the device prepare it is short
The method for strengthening element.
Background technique
Cycocel abbreviation CCC, effective component are chlorination -2- ethyl trimethyl ammonium chloride, are that a kind of plant having many uses is raw
Long regulator can be used for wheat, rice, cotton, tobacco, corn and tomato etc., pass through each absorbed organ of plant and plant
Intracorporal gibberellin works, and inhibits cell elongation, but do not influence cell division, inhibits cauline leaf growth without influencing sexual organ
Development.And cycocel can be used in mixed way with a variety of non-alkaline pesticides, micro- fertilizer, be easy to be degraded by enzymes in the soil, to rear stubble
Crop has no adverse effects.It is domestic at present that cycocel is mainly produced using autoclave discontinuum, i.e., equipped with excessive dichloroethanes
It is passed through front three amine gas in reaction kettle, under certain temperature and pressure, generates trimethylamine and dichloroethanes fast reaction short strong
Element, but gas-liquid mass transfer is poor, and trimethylamine fails to react completely, and reacting is exothermic reaction, needs to remove heat in time.Therefore exist
It often will appear reaction kettle body product in cycocel production process greatly, heat transfer effect is poor, and the reaction time is long, and impurity content height etc. is asked
Topic.
Reaction kettle is to have the rustless steel container physically or chemically reacted, carries out container according to different process conditions demands
Structure design is configured with parameter reaction kettle, and design condition, process, inspection and manufacture, examination are needed according to Its Relevant Technology Standards, with reality
The mixture response function of heating, evaporation, cooling and low high speed that existing technique requires.Reaction kettle cooling system using cooling coil into
Row is furnished with the inlet and outlet of cooling media on cooling coil.There are many media used, there is cooling water, liquid nitrogen, outer circulation cooling
Liquid etc..It for the installation site of cooling coil, is mounted on inside reaction kettle under normal conditions, for reducing the temperature for reacting interior material
Degree.And outside can be placed under conditions of requiring for material large viscosity or agitating paddle form to coil pipe: for matchmaker
Body, as heat source in the case where, cooling coil can be placed in media, and will considering for Resistant heating is specific
Depending on situation, but whether being which kind of form should all consider heating effect and cooling effect.Also have and be welded on cooling coil
The form of half coil pipe is formed outside autoclave body.
Summary of the invention
The present invention provides a kind of low power consumings, efficient multipoles reactors.
In order to achieve the above objectives, concrete scheme of the invention is as follows:
A kind of multipoles reactors, it is characterised in that: including the head tank one being sequentially connected in series, mixing vessel and n grades it is anti-
Answer kettle.The multipoles reactors further include head tank two, and the head tank one and head tank two are arranged in parallel；Wherein n is
The integer of 3-10.Pressure reducing valve is provided between the (n-1)th order reaction kettle and the n-th order reaction kettle.
To improve reaction efficiency, promote fully reacting.The reaction kettle is enamel reaction still or metal steel bomb.
The reactor volume is 1000 ~ 8000L；N is 3-5.
For the temperature for controlling reaction kettle, timely heat transfer, cooling system built in the reaction kettle, refrigerant is water.
The present invention also provides a kind of methods for preparing cycocel using multipoles reactors serialization, have production
Stablize, the reaction time is short, the high feature of yield.
In order to achieve the above objectives, concrete scheme of the invention is as follows:
A method of cycocel is prepared using multipoles reactors, comprising the following steps:
Dichloroethanes is added in head tank one, trimethylamine is added in head tank two；Above two raw material is passed through static state
Mixer in be sufficiently mixed；
Temperature in the multipoles reactors first order reaction kettle is 80 ~ 100 DEG C, in 2 ~ n order reaction kettle
After temperature reaches 120 DEG C by gradient increased temperature to temperature, 120 DEG C of temperature of holding is constant in subsequent reactions kettle,
By in mixer dichloroethanes and trimethylamine be successively passed through n-1 order reaction kettle；After pressure reducing valve depressurizes, enter
N-th order reaction kettle.
Cycocel will can be obtained after centrifugation drying by n order reaction kettle feed liquid, the dichloroethanes mother liquor after centrifugation is passed through
Head tank one is recycled.
To promote fully reacting, the trimethylamine: the flow-rate ratio of dichloroethanes is 1:8 ~ 15.Reaction kettle is using volume
1/2 ~ 4/5 volume；Reactor pressure is 0.2 ~ 1.0MPa.
The prior art uses single reaction kettle, low in initial reaction stage reaction kettle reaction temperature, and reaction is mild, cooling water flow
Smaller, with the progress of reaction, temperature is increased rapidly, and reaction acutely, needs the heat of timely transfer reaction generation, so that
Cooling water amount is larger.In view of the above-mentioned problems, the present invention is that a kind of continuous production is short strong using multistage autoclave series connection successive reaction
The technique of element, can be effectively solved the loss of the energy generated in the production of traditional batch autoclave, the maintenance of equipment, and production is coordinated
A series of problems, such as, it is conducive to control, it is easy to produce, energy loss is reduced, enterprise profit is increased.Specifically have the beneficial effect that:
1. raw material material is reacted in serialization plural serial stage reaction unit, reaction process carries out step by step, the reaction time
Shorten；Trimethylamine does not need vaporization and is directly entered reaction kettle, and liquid-liquid transfer is abundant, and trimethylamine can be converted completely, and material exists
The high temperature lower residence time is short, and impurity content is low, and the cycocel raw medicine of 99% or more high-purity of content can be made.
2. the production of serialization plural serial stage reaction unit is stablized, the reaction time is short, high production efficiency, can increase substantially
The production yields of cycocel raw medicine.
3. overall process continuous reaction, it is possible to implement the automation DCS of overall process is controlled, stable product quality, and labour is strong
It spends low, while having preferable effects of energy saving and emission reduction again.
Detailed description of the invention
Fig. 1 is the structural diagram of the present invention.
Label declaration
Head tank 1, head tank 22, mixing vessel 3, first order reaction kettle 4, the second reaction kettle 5, third reaction kettle 6.
Specific embodiment
Reaction kettle is purchased from Zibo Wo Tai chemical machinery Co., Ltd.
Embodiment 1
A kind of multipoles reactors, the multipoles reactors are 3 grades of tandem reaction kettles.As shown in Figure 1, include according to
Secondary concatenated head tank 1, mixing vessel 3, first order reaction kettle 4, the second reaction kettle 5, third reaction kettle 6.The multistage string
Joining reaction kettle further includes head tank 22, and the head tank 1 and head tank 22 are arranged in parallel, and are placed in front of mixing vessel 3.Institute
State setting pressure reducing valve 7 between the second reaction kettle 5 and third reaction kettle 6.The bottom of the first order reaction kettle 4 and the second reaction kettle
5 connections, 5 bottom of the second reaction kettle and third reaction kettle 6 connect.The first, second, third order reaction kettle volume is
1000L is provided with cooling device on the first, second, third order reaction kettle.Cooling system built in the reaction kettle,
Refrigerant is water.The first, second, third order reaction kettle interior reaction temperature is 100 DEG C, 120 DEG C, 120 DEG C.
A method of cycocel is prepared using 3 grades of tandem reaction kettles, comprising the following steps:
Dichloroethanes is added in head tank 1, trimethylamine is added in head tank 22 for the first step；By above two raw material
It is passed through in static mixer 3 and is sufficiently mixed, the trimethylamine: the flow-rate ratio of dichloroethanes is 1:8.
Second step, by mixer 3 dichloroethanes and trimethylamine be passed through first order reaction kettle 4, open first, second,
Cooling device on third level reaction kettle, adjusting first order reaction kettle reaction temperature is 100 DEG C,
Third step, by the raw material in first order reaction kettle 4, from bottom, extraction enters second level reaction kettle 5, the second level
5 reaction temperature of reaction kettle is 120 DEG C
4th step will produce anti-into the third level after pressure reducing valve 7 is slowly decompressed to normal pressure from 5 bottom of second level reaction kettle
Kettle 6 is answered,
4th step, 99.6% cycocel raw medicine can be obtained in the feed liquid of third level reaction kettle 6 after centrifugation drying, after centrifugation
Dichloroethanes mother liquor be passed through head tank 1 and recycled.
Reaction pressure in the first, second, third order reaction kettle is 0.3MPa.Described first, second, third grade anti-
Answer kettle is 1/2 volume using volume.
Embodiment 2
A kind of multipoles reactors, other are distinguished as described in Example 1 and are the continuous multi-stage tandem reaction kettle dress
5 grades of tandem reaction kettles are set to, wherein first order reaction kettle interior reaction temperature is 90 DEG C, and the temperature of the 2nd ~ 5 order reaction kettle presses 10 DEG C
Gradient increased temperature, until keeping 120 DEG C of temperature constant (the i.e. temperature of 5 order reaction kettles in subsequent reactions kettle after temperature reaches 120 DEG C
Degree is followed successively by 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C, 120 DEG C)；The reactor volume is 2000L.
A method of cycocel being prepared using 5 grades of tandem reaction kettles, dichloroethanes, head tank are added in head tank one
Trimethylamine is added in two；Above two raw material is passed through in static mixer and is sufficiently mixed；
By in mixer dichloroethanes and trimethylamine be successively passed through preceding 4 order reaction kettle；After pressure reducing valve depressurizes, enter
5th order reaction kettle.
99.7% cycocel raw medicine will can be obtained after centrifugation drying by 5 order reaction kettle feed liquids, two chloroethenes after centrifugation
Alkane mother liquor is passed through head tank one and is recycled.
Reaction pressure in the 5 order reaction kettle is 0.5MPa；The trimethylamine: the flow-rate ratio of dichloroethanes is 1:10.
The reaction kettle is 3/5 volume using volume.
Embodiment 3
A kind of multipoles reactors, other are distinguished as described in Example 1 and are the continuous multi-stage tandem reaction kettle dress
8 grades of tandem reaction kettles are set to, the first order reaction kettle interior reaction temperature is 80 DEG C, and the temperature of the 2nd ~ 8 order reaction kettle is by 7 DEG C
Gradient increased temperature, until keeping 120 DEG C of temperature constant (the i.e. temperature of 8 order reaction kettles in subsequent reactions kettle after temperature reaches 120 DEG C
It is followed successively by 80 DEG C, 87 DEG C, 94 DEG C, 101 DEG C, 108 DEG C, 115 DEG C, 120 DEG C, 120 DEG C).The reactor volume is 3000L.
A method of cycocel being prepared using 8 grades of tandem reaction kettles, dichloroethanes, head tank are added in head tank one
Trimethylamine is added in two；Above two raw material is passed through in static mixer and is sufficiently mixed；
By in mixer dichloroethanes and trimethylamine be successively passed through preceding 7 order reaction kettle；After pressure reducing valve depressurizes, enter
8th order reaction kettle.
99.5% cycocel raw medicine will can be obtained after centrifugation drying by 8 order reaction kettle feed liquids, two chloroethenes after centrifugation
Alkane mother liquor is passed through head tank one and is recycled.
Reaction pressure in the 8 order reaction kettle is 0.7MPa；The trimethylamine: the flow-rate ratio of dichloroethanes is 1:12.
The reaction kettle is 7/10 volume using volume.
Embodiment 4
A kind of multipoles reactors, other are distinguished as described in Example 1 and are the continuous multi-stage tandem reaction kettle dress
10 grades of series connection are set to, the reaction temperature of the first order reaction kettle is 80 DEG C, and the temperature of the 2nd ~ 10 order reaction kettle presses 6 DEG C of gradient
Heating, until keeping 120 DEG C of temperature after temperature reaches 120 DEG C, in subsequent reactions kettle, constant (i.e. the temperature of 10 order reaction kettles is successively
It is 80 DEG C, 86 DEG C, 92 DEG C, 98 DEG C, 104 DEG C, 110 DEG C, 116 DEG C, 120 DEG C, 120 DEG C, 120 DEG C).The reactor volume is
5000L。
A method of cycocel being prepared using 10 grades of tandem reaction kettles, dichloroethanes, raw material are added in head tank one
Trimethylamine is added in tank two；Above two raw material is passed through in static mixer and is sufficiently mixed；
By in mixer dichloroethanes and trimethylamine be successively passed through preceding 9 order reaction kettle；After pressure reducing valve depressurizes, enter
10th order reaction kettle.
99.3% cycocel raw medicine will can be obtained after centrifugation drying by 10 order reaction kettle feed liquids, the dichloro after centrifugation
Ethane mother liquor is passed through head tank one and is recycled.
Reaction pressure in the 10 order reaction kettle is 0.9MPa, and the trimethylamine: the flow-rate ratio of dichloroethanes is 1:15.
The reaction kettle is 4/5 volume using volume.
Above specific embodiment is only the preferred embodiment of this creation, all in this wound not to limit this creation
Any modification, equivalent substitution, improvement and etc. done within the spirit and principle of work, should be included in this creation protection scope it
It is interior.
Claims (8)
1. a kind of method for preparing cycocel using multipoles reactors, it is characterised in that: using multipoles reactors and
Following steps:
The multipoles reactors include the head tank one being sequentially connected in series, mixing vessel and n order reaction kettle；
The multipoles reactors further include head tank two, and the head tank one and head tank two are arranged in parallel；Wherein n is 3-
10 integer；Pressure reducing valve is provided between the (n-1)th order reaction kettle and the n-th order reaction kettle；
The step are as follows:
Dichloroethanes is added in head tank one, trimethylamine is added in head tank two；Above two raw material is passed through static mix
It is sufficiently mixed in clutch；
Temperature setting in the multipoles reactors first order reaction kettle is 80 ~ 100 DEG C, in 2 ~ n order reaction kettle
After temperature reaches 120 DEG C by gradient increased temperature to temperature, 120 DEG C of temperature of holding is constant in subsequent reactions kettle；
By in mixer dichloroethanes and trimethylamine be successively passed through n-1 order reaction kettle；After pressure reducing valve depressurizes, into n-th
Order reaction kettle；
Cycocel will can be obtained after centrifugation drying by n order reaction kettle feed liquid, the dichloroethanes mother liquor after centrifugation is passed through raw material
Tank one is recycled.
2. the method according to claim 1 for preparing cycocel using multipoles reactors, which is characterized in that described three
Methylamine: the flow-rate ratio of dichloroethanes is 1:8 ~ 15.
3. the method according to claim 1 for preparing cycocel using multipoles reactors, it is characterised in that: reaction kettle
Using volume be 1/2 ~ 4/5 volume.
4. the method according to claim 1 for preparing cycocel using multipoles reactors, it is characterised in that: reaction kettle
Pressure is 0.2 ~ 1.0MPa.
5. the method according to claim 1 for preparing cycocel using multipoles reactors, it is characterised in that: described
Reaction kettle is enamel reaction still or metal steel bomb.
6. the method according to claim 1 for preparing cycocel using multipoles reactors, it is characterised in that: described
Reactor volume is 1000 ~ 8000L.
7. the method according to claim 1 for preparing cycocel using multipoles reactors, it is characterised in that: n 3-
5。
8. the method according to claim 1 for preparing cycocel using multipoles reactors, it is characterised in that: described
Cooling system built in reaction kettle, refrigerant are water.
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| CN201810562564.2A CN108499508B (en) | 2018-06-04 | 2018-06-04 | A kind of multipoles reactors and the method for preparing cycocel using the device |
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| CN201810562564.2A CN108499508B (en) | 2018-06-04 | 2018-06-04 | A kind of multipoles reactors and the method for preparing cycocel using the device |
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| CN110511148A (en) * | 2019-09-12 | 2019-11-29 | 郑州信联生化科技有限公司 | The preparation and its application of one plant growth regulators |
| CN112973607A (en) * | 2021-04-19 | 2021-06-18 | 鹤壁全丰生物科技有限公司 | Continuous production device and process of chlormequat chloride |
| CN114539076A (en) * | 2022-03-28 | 2022-05-27 | 苏州市晶协高新电子材料有限公司 | Continuous synthesis device and process of dimethyl diallyl ammonium chloride |
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| CN101717339A (en) * | 2009-12-08 | 2010-06-02 | 江苏扬农化工集团有限公司 | Double quaternary ammonium base compound and preparation method as well as application thereof |
| CN102477018B (en) * | 2010-11-30 | 2013-08-14 | 中国科学院大连化学物理研究所 | Continuous production device for preparing epichlorohydrin by using hydrogen peroxide to oxidize chloropropene under conditions of normal pressure and no solvent |
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Address after: 359 Jiangzhong Road, Doumen street, Yuecheng District, Shaoxing City, Zhejiang Province Patentee after: SHAOXING DONGHU HIGH-TECH Co.,Ltd. Address before: 312000 Doumen Town, Yuecheng District, Shaoxing, Zhejiang Patentee before: SHAOXING DONGHU HIGH-TECH Co.,Ltd. |