CN109757482A - A kind of continuous preparation method of pesticide dimethylamine salt aqua - Google Patents

A kind of continuous preparation method of pesticide dimethylamine salt aqua Download PDF

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Publication number
CN109757482A
CN109757482A CN201711095993.5A CN201711095993A CN109757482A CN 109757482 A CN109757482 A CN 109757482A CN 201711095993 A CN201711095993 A CN 201711095993A CN 109757482 A CN109757482 A CN 109757482A
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China
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kettle
dimethylamine
pesticide
preparation
original medicine
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CN201711095993.5A
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Chinese (zh)
Inventor
孙国庆
侯永生
李遵亮
胡义山
周长涛
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Shandong Runbo Biological Technology Co Ltd
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Shandong Runbo Biological Technology Co Ltd
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Priority to CN201711095993.5A priority Critical patent/CN109757482A/en
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Abstract

The present invention provides a kind of continuous preparation methods of pesticide dimethylamine salt aqua, it include: to mix pesticide original medicine in preparing kettle with water, dimethylamine gas is continually fed into according to the reaction ratio of pesticide original medicine and dimethylamine gas, it is continually fed into pesticide original medicine and water again, the full rear overflow of kettle is prepared to next preparation kettle, until the last one, which prepares kettle overflow, goes out material, the material is pesticide dimethylamine salt aqua;It is described prepare kettle number >=2 and be arranged in series.Preparation method provided by the present application can realize that automatic control continuous production, dimethylamine gas are directly passed through by pressure control, non-volatile problem, and environmental protection is controllable;Personnel's not contacting material substantially improves safety, and automatic control level is high, and production capacity is high, and primary verification qualification rate is high, and parameter is easy to control.

Description

A kind of continuous preparation method of pesticide dimethylamine salt aqua
Technical field
The present invention relates to preparation technique of pesticide field more particularly to a kind of serialization preparation sides of pesticide dimethylamine salt aqua Method.
Background technique
Pesticide in use be usually effective component play a role, and agriculture the effective elements of the medicine in forming salt sometimes Using effect is preferable, and into salt aqua dosage form again as first choice, therefore the production of aqueous pesticide solution is particularly important.The production of aqua exists The country be according to intermittent preparation produce carry out, and in the whole world also with intermittence production based on.
Intermittence production is there are human cost height, and production capacity is low, the uncontrollable problem of quality index.Therefore, pesticide water at present The production of agent needs the serialization by production, changes the adding manner of material and prepares the set-up mode of kettle, by chain Control makes its aqua serialization, finally solves the problems, such as that cost, production capacity and quality index are uncontrollable.
Summary of the invention
Present invention solves the technical problem that being to provide a kind of continuous preparation method of pesticide dimethylamine salt aqua, this Shen The preparation method that please be provided can realize automatic control serialization.
In view of this, this application provides a kind of continuous preparation methods of pesticide dimethylamine salt aqua, comprising:
Pesticide original medicine is mixed in preparing kettle with water, is persistently led to according to the reaction ratio of pesticide original medicine and dimethylamine gas Enter dimethylamine gas, then be continually fed into pesticide original medicine and water, prepares the full rear overflow of kettle to next preparation kettle, until the last one is matched Kettle overflow processed goes out material, and the material is pesticide dimethylamine salt aqua;It is described prepare kettle number >=2 and be arranged in series.
Preferably, it is total intake that the opportunity for being continually fed into pesticide original medicine and water, which is the intake of dimethylamine gas, 80%~90%.
Preferably, the pesticide original medicine is 2,4- dichlorphenoxyacetic acid, dicamba or glyphosate.
Preferably, the molar ratio of the pesticide original medicine and the dimethylamine gas is 1:(0.9~1.6).
Preferably, the molar ratio of the pesticide original medicine and the dimethylamine gas is 1:(1.0~1.3).
Preferably, the pressure of the dimethylamine gas is 0.01~0.09MPa, and the flow velocity of the dimethylamine gas is 0.5 ~3T/h.
Preferably, the pressure of the dimethylamine gas is 0.03~0.08MPa, and the flow velocity of the dimethylamine gas is 0.6 ~1.8T/h.
Preferably, the number for preparing kettle is 2~5.
Preferably, the height for preparing kettle successively reduces.
Preferably, it is prepared in kettle at the last one and auxiliary agent is added.
This application provides a kind of continuous preparation methods of pesticide dimethylamine salt aqua, comprising: by pesticide original medicine and water It is mixed in preparing kettle, is continually fed into dimethylamine gas according to the reaction ratio of pesticide original medicine and dimethylamine gas, then persistently lead to Enter pesticide original medicine and water, prepares the full rear overflow of kettle to next preparation kettle, until the last one, which prepares kettle overflow, goes out material, the object Material is pesticide dimethylamine salt aqua;It is described prepare kettle number >=2 and be arranged in series.Preparation method provided by the present application can be realized Automatic control continuous production, dimethylamine gas are directly passed through by pressure control, non-volatile problem, and environmental protection is controllable;Personnel are substantially not Contacting material improves safety, and automatic control level is high, and production capacity is high, and primary verification qualification rate is high, and parameter is easy to control.
Detailed description of the invention
Fig. 1 is the continuous preparation method flow diagram of pesticide dimethylamine salt aqua provided by the invention.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still It should be appreciated that these descriptions are only further explanation the features and advantages of the present invention, rather than to the claims in the present invention Limitation.
For the intermittent production operation of aqueous pesticide solution in the prior art, personnel safety is low, product production capacity is low, quality mark The problem of quasi- controlling difference, the embodiment of the invention discloses a kind of continuous preparation method of pesticide dimethylamine salt aqua, the party Method can realize the continuous production of pesticide dimethylamine salt aqua, and do not need personnel and directly operate, highly-safe, and aqua is prepared Conveniently, accuracy rate is higher.The preparation flow of the application pesticide dimethylamine salt aqua is as shown in Figure 1, specifically, include:
Pesticide original medicine is mixed in preparing kettle with water, is persistently led to according to the reaction ratio of pesticide original medicine and dimethylamine gas Enter dimethylamine gas, then be continually fed into pesticide original medicine and water, prepares the full rear overflow of kettle to next preparation kettle, until the last one is matched Kettle overflow processed goes out material, and the material is pesticide dimethylamine salt aqua;It is described prepare kettle number >=2 and be arranged in series.
In the preparation process of pesticide dimethylamine salt aqua, the pesticide original medicine of the application preferred pin pair is 2,4- Dichlorophenoxy Acetic acid, dicamba or glyphosate, i.e. the application are prepared for 2,4- dichlorphenoxyacetic acid dimethylamine salt aqua, wheat by the above method Grass fear dimethylamine salt aqua or glyphosate dimethylamine salt aqua.In order to guarantee preparation aqueous pesticide solution meet reaction proportion and The application demand of aqueous pesticide solution, for above-mentioned effective component, the molar ratio of the pesticide original medicine and dimethylamine gas is 1:(0.9 ~1.6), in a particular embodiment, the molar ratio of the pesticide original medicine and dimethylamine gas is 1:(1.0~1.3).
Specifically, pesticide original medicine and soft water are added to preparation first in the preparation process of pesticide dimethylamine salt aqua It is mixed in kettle, and opens stirring;The kettle of preparing is the vessel well known to those skilled in the art for preparing pesticide, to this application Without particularly limiting.
It is added in pesticide original medicine and soft water to after preparing kettle, then starts to be passed through dimethylamine gas;In entire configuration process In, dimethylamine gas is continually fed into preparation kettle, and being passed through for dimethylamine gas meets above-mentioned molar ratio, to guarantee pesticide original Medicine is sufficiently reacted with dimethylamine gas.It is controlled during being passed through dimethylamine gas by pressure pressure tank, so that dimethylamine The pressure of gas is 0.01~0.09MPa, and in a particular embodiment, the pressure of the dimethylamine gas is 0.03~0.08MPa, More specifically, the pressure of the dimethylamine gas is 0.01~0.03MPa, 0.03~0.04MPa or 0.07~0.08MPa.Institute The flow velocity for stating dimethylamine gas is 0.5~3T/h, and in a particular embodiment, the flow velocity of the dimethylamine gas is 0.6~1.8T/ h.The restriction of above-mentioned dimethylamine gas pressure and flow velocity just can guarantee the dimethylamine amount and effective component for eventually entering into and preparing in kettle Match, reach the delay reaction time in kettle carries out next preparation kettle again.The process for preparing kettle is passed through in dimethylamine gas In, pesticide original medicine and dimethylamine gas are constantly in reactiveness, after dimethylamine gas is passed through a period of time, specially diformazan When amine gas intake is the 80%~90% of total amount, starts to be continually fed into pesticide original medicine and soft water, pesticide original medicine is added herein Specifically as follows with the proportion of soft water: the addition of pesticide original medicine according to the addition of the reaction ratio of dimethylamine gas, it is soft The addition of water is consistent with the concentration of the aqueous pesticide solution finally configured.The soft water of the application divides in the manner described above with pesticide original medicine It criticizes and is added, if being added at one time it cannot be guaranteed that ensured sustained development prepares and reaction effect, with being slowly added into for effective component, material Next preparation kettle is more and more overflowed to, if being added at one time, then it cannot be guaranteed that residence time in kettle.
With the progress of reaction, it is continuously added into pesticide original medicine and soft water, until first preparation kettle is full.The application is provided with Multiple concatenated preparation kettles, in order to which the material for being conducive to overflow is directly entered next preparation kettle, the multiple height for preparing kettle It is preferred that successively reducing.In this application, preferably concatenated number >=2 of preparation kettle, in a particular embodiment, the preparation kettle Number be 2~5.With the progress of reaction and the addition of raw material, after first preparation kettle is full, continue in first preparation kettle In be passed through dimethylamine gas and corresponding pesticide original medicine and soft water, then react after material be constantly spilled over to next match Kettle processed, until the material of spilling is pesticide dimethylamine salt aqua after the last one prepares kettle completely.In order to make pesticide dimethylamine salt Aqua is more conducive to use, and further includes auxiliary agent in the pesticide dimethylamine salt aqua, the application is preferably in the last one preparation kettle Auxiliary agent is added, so that it includes auxiliary agent that the last one, which is prepared in the material that overflow goes out in kettle, i.e., includes in pesticide dimethylamine salt aqua Auxiliary agent.
This application provides a kind of continuous preparation methods of pesticide dimethylamine salt aqua, are to continue dimethylamine gas Be passed through the water slurry of effective component, by prepare kettle series connection, raw medicine and water and dimethylamine according to a certain ratio, persistently plus Enter, sustained response, by the control to pressure, flow and proportion, obtains qualified dimethylamine aqua product, whole operation mistake Cheng Junwei automatic control, the dimethylamine salt aqua continuous production that personnel can be realized by control room, is waved to change dimethylamine Hair, personnel cost is high, and safety is low, and production capacity is low, the uncontrollable problem of quality.
For a further understanding of the present invention, below with reference to embodiment to the system of pesticide dimethylamine salt aqua provided by the invention Preparation Method is described in detail, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
3.59T soft water is added to 10KL to prepare in kettle, then by 5.25T 96%2,4- dichlorphenoxyacetic acid raw medicine is added To preparing in kettle, stirring is opened, starts to be passed through 0.92T dimethylamine gas, flow control is controlled in 1.2T/h, pressure in 0.07- 0.08MPa;When logical dimethylamine is in 40min, it is slowly added into soft water and 2,4- dichlorphenoxyacetic acid raw medicine (is delivered to by auger Prepare kettle), the molar ratio of effective component and dimethylamine is 1:1.03, i.e., every addition 1T raw medicine, must there is 0.21T dimethylamine to be passed through with And 0.686T water is added;With continuing for reaction, soft water and raw medicine are continuously added, when reaching total amount 10T, by high potential difference It overflows in second preparation kettle, after expiring with second kettle, third preparation kettle is overflowed to, until third preparation kettle overflow Material out, this material are qualified 2,4- dichlorphenoxyacetic acid dimethylamine salt, 60% aqua product.
Embodiment 2
4.902T soft water is added to 10KL to prepare in kettle, then 97% dicamba raw medicine of 4.258T is added to preparation kettle In, stirring is opened, starts to be passed through 0.84T dimethylamine gas, flow control is controlled in 0.5T/h, pressure in 0.01-0.02MPa; When logical dimethylamine is in 90min, be slowly added into soft water and dicamba raw medicine (be delivered to by auger and prepare kettle), effective component with The molar ratio of dimethylamine is 1:1.00, i.e., every addition 1T raw medicine must have 0.23T dimethylamine to be passed through and be uniformly added into 1.151T water; With continuing for reaction, soft water and raw medicine are continuously added, when reaching total amount 10T, second is overflowed to by high potential difference and matches In kettle processed, as the full rear overflow of second kettle goes out material, this material is qualified 50% aqua product of dicamba dimethylamine salt.
Embodiment 3
4.182T soft water is added to 10KL to prepare in kettle, then 95% glyphosate technicals of 4.158T are added to preparation kettle In, stirring is opened, starts to be passed through 1.25T dimethylamine gas, flow control is controlled in 0.6T/h, pressure in 0.03-0.04MPa; When logical dimethylamine is in 90min, be slowly added into soft water and glyphosate technicals (be delivered to by auger and prepare kettle), effective component with The molar ratio of dimethylamine is 1:1.2, i.e., every addition 1T raw medicine must have 0.30T dimethylamine to be passed through and be uniformly added into 1.007T water;With Reaction continue, continuously add soft water and raw medicine, when reaching total amount 10T, overflow to second preparation by high potential difference In kettle, overflow goes out material into third kettle after second kettle is full, successively the 5th preparation kettle of most Zhongdao, this is prepared is added in kettle 0.41T auxiliary agent, until overflow goes out material, this material is qualified 50.4% aqua product of glyphosate dimethylamine salt.
Embodiment 4
2.873T soft water is added to 10KL to prepare in kettle, then by 5.927T 96%2,4- dichlorphenoxyacetic acid raw medicine adds Enter to preparing in kettle, open stirring, starts to be passed through 1.2T dimethylamine gas, flow control is controlled in 1.2T/h, pressure in 0.07- 0.08MPa;When logical dimethylamine is in 50min, it is slowly added into soft water and 2,4- dichlorphenoxyacetic acid raw medicine (is delivered to by auger Prepare kettle), the molar ratio of effective component and dimethylamine is 1:1.03, i.e., every addition 1T raw medicine, must there is 0.21T dimethylamine to be passed through with And 0.686T water is added;With continuing for reaction, soft water and raw medicine are continuously added, when reaching total amount 10T, by high potential difference It overflows in second preparation kettle, after expiring with second kettle, third preparation kettle is overflowed to, until third preparation kettle overflow Material out, this material are qualified 2,4- dichlorphenoxyacetic acid dimethylamine salt, 70% aqua product.
Embodiment 5
5.559T soft water is added to 10KL to prepare in kettle, then by 3.677T 96%2,4- dichlorphenoxyacetic acid raw medicine adds Enter to preparing in kettle, open stirring, starts to be passed through 0.764T dimethylamine gas, flow control exists in 1.2T/h, pressure control 0.07-0.08MPa;When logical dimethylamine is in 32min, it is slowly added into soft water and 2,4- dichlorphenoxyacetic acid raw medicine (passes through auger It is delivered to and prepares kettle), the molar ratio of effective component and dimethylamine is 1:1.03, i.e., every addition 1T raw medicine must have 0.21T dimethylamine It is passed through and 0.686T water is added;With continuing for reaction, soft water and raw medicine are continuously added, when reaching total amount 10T, is passed through High potential difference overflows in second preparation kettle, after expiring with second kettle, overflows to third preparation kettle, until third is prepared Kettle overflow goes out material, this material is qualified 2,4- dichlorphenoxyacetic acid dimethylamine salt, 42.5% aqua product.
Embodiment 6
5.62T soft water is added to 10KL to prepare in kettle, then 97% dicamba raw medicine of 3.67T is added to and is prepared in kettle, Stirring is opened, starts to be passed through 0.728T dimethylamine gas, flow control is controlled in 0.5T/h, pressure in 0.01-0.02MPa;When Logical dimethylamine is slowly added into soft water and dicamba raw medicine (be delivered to by auger and prepare kettle), effective component and two in 80min The molar ratio of methylamine is 1:1.00, i.e., every addition 1T raw medicine must have 0.23T dimethylamine to be passed through and be uniformly added into 1.151T water;With Reaction continue, continuously add soft water and raw medicine, when reaching total amount 10T, overflow to second preparation by high potential difference In kettle, as the full rear overflow of second kettle goes out material, this material is qualified 42.8% aqua product of dicamba dimethylamine salt.
Embodiment 7
5.208T soft water is added to 10KL to prepare in kettle, then 95% glyphosate technicals of 3.684T are added to preparation kettle In, stirring is opened, starts to be passed through 1.108T dimethylamine gas, flow control is controlled in 0.6T/h, pressure in 0.03-0.04MPa; When logical dimethylamine is in 80min, be slowly added into soft water and glyphosate technicals (be delivered to by auger and prepare kettle), effective component with The molar ratio of dimethylamine is 1:1.2, i.e., every addition 1T raw medicine must have 0.30T dimethylamine to be passed through and be uniformly added into 1.007T water;With Reaction continue, continuously add soft water and raw medicine, when reaching total amount 10T, overflow to second preparation by high potential difference In kettle, overflow goes out material into third kettle after second kettle is full, successively the 5th preparation kettle of most Zhongdao, this is prepared is added in kettle 0.40T auxiliary agent, until overflow goes out material, this material is qualified 44.3% aqua product of glyphosate dimethylamine salt
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one The widest scope of cause.

Claims (10)

1. a kind of continuous preparation method of pesticide dimethylamine salt aqua, comprising:
Pesticide original medicine is mixed in preparing kettle with water, is continually fed into two according to the reaction ratio of pesticide original medicine and dimethylamine gas Methylamine gas, then it is continually fed into pesticide original medicine and water, the full rear overflow of kettle is prepared to next preparation kettle, until the last one prepares kettle Overflow goes out material, and the material is pesticide dimethylamine salt aqua;It is described prepare kettle number >=2 and be arranged in series.
2. continuous preparation method according to claim 1, which is characterized in that pesticide original medicine and the water of being continually fed into Opportunity is 80%~90% that the intake of dimethylamine gas is total intake.
3. continuous preparation method according to claim 1, which is characterized in that the pesticide original medicine is 2,4- Dichlorophenoxy Acetic acid, dicamba or glyphosate.
4. continuous preparation method according to claim 1, which is characterized in that the pesticide original medicine and the dimethylamine gas The molar ratio of body is 1:(0.9~1.6).
5. continuous preparation method according to claim 4, which is characterized in that the pesticide original medicine and the dimethylamine gas The molar ratio of body is 1:(1.0~1.3).
6. continuous preparation method according to claim 1, which is characterized in that the pressure of the dimethylamine gas is 0.01 ~0.09MPa, the flow velocity of the dimethylamine gas are 0.5~3T/h.
7. continuous preparation method according to claim 6, which is characterized in that the pressure of the dimethylamine gas is 0.03 ~0.08MPa, the flow velocity of the dimethylamine gas are 0.6~1.8T/h.
8. continuous preparation method according to claim 1, which is characterized in that the number for preparing kettle is 2~5.
9. continuous preparation method according to claim 1, which is characterized in that the height for preparing kettle successively reduces.
10. described in any item continuous preparation methods according to claim 1~9, which is characterized in that in the last one preparation kettle Middle addition auxiliary agent.
CN201711095993.5A 2017-11-09 2017-11-09 A kind of continuous preparation method of pesticide dimethylamine salt aqua Pending CN109757482A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1365254A (en) * 1999-07-28 2002-08-21 孟山都技术有限公司 Process for making a downstream processable ammonium glyphosate paste
CN101723973A (en) * 2009-12-09 2010-06-09 浙江新安化工集团股份有限公司 Method for preparing glyphosate dimethylamine salt solid
CN102746194A (en) * 2012-07-19 2012-10-24 江苏扬农化工集团有限公司 Industrial production method for continuously preparing Dailon
US20130225407A1 (en) * 2004-08-19 2013-08-29 Monsanto Technology Llc Glyphosate salt herbicidal composition
CN107318883A (en) * 2017-07-14 2017-11-07 安徽嘉联生物科技有限公司 A kind of aqua for including glyphosate Mediben

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1365254A (en) * 1999-07-28 2002-08-21 孟山都技术有限公司 Process for making a downstream processable ammonium glyphosate paste
US20130225407A1 (en) * 2004-08-19 2013-08-29 Monsanto Technology Llc Glyphosate salt herbicidal composition
CN101723973A (en) * 2009-12-09 2010-06-09 浙江新安化工集团股份有限公司 Method for preparing glyphosate dimethylamine salt solid
CN102746194A (en) * 2012-07-19 2012-10-24 江苏扬农化工集团有限公司 Industrial production method for continuously preparing Dailon
CN107318883A (en) * 2017-07-14 2017-11-07 安徽嘉联生物科技有限公司 A kind of aqua for including glyphosate Mediben

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