CN110317152A - A kind of O- methyl-N methyl-N '-nitro isourea production method - Google Patents

A kind of O- methyl-N methyl-N '-nitro isourea production method Download PDF

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Publication number
CN110317152A
CN110317152A CN201910527330.9A CN201910527330A CN110317152A CN 110317152 A CN110317152 A CN 110317152A CN 201910527330 A CN201910527330 A CN 201910527330A CN 110317152 A CN110317152 A CN 110317152A
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China
Prior art keywords
methyl
light
temperature
continuous work
probe
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Inventor
周建锋
陈杨
欧阳兆辉
颜志斌
简理
朱传胜
夏勇
陈进
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QIANJIANG FANGYUAN TITANIUM CO Ltd
Qianjiang Yuan Da Chemical Co Ltd
Wuhan Qingjaing Chemical Huanggang Co Ltd
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QIANJIANG FANGYUAN TITANIUM CO Ltd
Qianjiang Yuan Da Chemical Co Ltd
Wuhan Qingjaing Chemical Huanggang Co Ltd
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Priority to CN201910527330.9A priority Critical patent/CN110317152A/en
Publication of CN110317152A publication Critical patent/CN110317152A/en
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
    • C07C273/18—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of substituted ureas
    • G—PHYSICS
    • G05—CONTROLLING; REGULATING
    • G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
    • G05D23/00—Control of temperature
    • G05D23/19—Control of temperature characterised by the use of electric means
    • G05D23/20—Control of temperature characterised by the use of electric means with sensing elements having variation of electric or magnetic properties with change of temperature

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Automation & Control Theory (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention belongs to high-molecular compound preparation technical fields, disclose a kind of O- methyl-N methyl-N '-nitro isourea production method, reaction solution are added in the cooling water of temperature control, crystallization；Cooling water is regulated and controled by temperature-controlling system, acquires ultrasonic probe operative scenario temperature data using the camera of temperature-controlling system；Acquire ultrasonic probe temperature data in real time using temperature sensor；Ultrasonic propagation velocity data are measured using the measuring device of temperature-controlling system；Ultrasonic probe refrigeration cool-down is operated using refrigerator；Adaptive matching operation is carried out to ultrasonic probe and ultrasonic device master unit using automatic adaptation program；Using alert device according to abnormal temperature data and alert notification；Utilize the ultrasonic probe operative scenario temperature data of display display acquisition.Temperature control instrument of the present invention can be carried out and alarm, and for temperature control in reaction at positive and negative 1 degree Celsius, product property and purity to production unanimously provide guarantee.

Description

A kind of O- methyl-N methyl-N '-nitro isourea production method
Technical field
The invention belongs to high-molecular compound preparation technical field more particularly to a kind of O- methyl-N methyl-N '-nitros Isourea production method.
Background technique
Currently, the immediate prior art:
O- methyl-N-methyl-N '-nitro isourea category pesticide intermediate, spreads out mainly for the preparation of the guanidine with insecticidal activity The main intermediate of biology and dinotefuran.Molecular formula is as follows:
O- methyl-N-methyl-N '-nitro isourea obtains O- by acidolysis, hydrolysis by dimethyl suflfate and urea reaction Methyl-isourea disulfate (O- methyl-isourea disulfate nitrification, again methylamine reaction preparation.105% acid of primary raw material, 98% Acid, methoxyl-isourea hydrosulfate, nitric acid and methylamine water solution, the dilute sulfuric acid of by-product concentration 40%).
In prior art production, most of temperature control method in reaction process is adjusted by simple instrument.
In conclusion problem of the existing technology is:
Current country O- methyl-N-methyl-N '-nitro isourea production capacity much can not meet the market demand, existing O- In methyl-N-methyl-N '-nitro isourea production process, a large amount of wastes can be generated, seriously polluted, Simultaneous Nitrification reaction, first Glycosylation reaction process reaction yield is low, and preparation efficiency is not high, at high cost.
It is poor to rice water weevil control efficiency.
During the reaction in temperature control method, if temperature control instrument will cause very big harm to reaction once breaking down, And not can be carried out timely alarm, for reaction in temperature control error, the prior art substantially at positive and negative 5 degrees Celsius, it is this substantially The degree temperature difference can impact the product property and purity of production.
Summary of the invention
In view of the problems of the existing technology, the present invention provides a kind of O- methyl-N methyl-N '-nitro isourea productions Method.
The invention is realized in this way a kind of O- methyl-N methyl-N '-nitro isourea production method, the O- methyl-N Methyl-N '-nitro isourea production method includes: O- methyl-isourea disulfate and oleum, concentrated nitric acid nitration reaction, is obtained To reaction solution.Reaction solution is added in the cooling water of temperature control, crystallization.Cooling water is regulated and controled by temperature-controlling system, utilizes temperature control The camera of system acquires ultrasonic probe operative scenario temperature data.Acquire ultrasonic probe temperature in real time using temperature sensor Data.Ultrasonic propagation velocity data are measured using the measuring device of temperature-controlling system.Freezed using refrigerator to ultrasonic probe and is dropped Temperature operation.
Adaptive matching operation is carried out to ultrasonic probe and ultrasonic device master unit using automatic adaptation program.Utilize police Report equipment according to abnormal temperature data and alert notification.
Utilize the ultrasonic probe operative scenario temperature data information of display display acquisition.
Further, the ultrasonic velocity measurement module measurement method includes:
(1) the ultrasonic propagation velocity V under test specimen room temperature state is obtained by measuring device0。
(2) test specimen is heated, by ultrasound method, test specimen tiThe ultrasonic propagation time t at momenti,exp。
(3) Optimized model of ultrasonic propagation velocity measurement is established.The objective function of optimization are as follows:
Wherein: V is ultrasonic propagation velocity to be measured.ti,calThe t being calculated for numerical valueiThe ultrasonic wave at moment is propagated Time, the time of measuring ordinal number that subscript i is indicated, N indicate total time of measuring points.L is the length that test specimen is tested direction.
Constraint condition are as follows:
f(Vj)=V0
Wherein: k, C and ρ are respectively thermal coefficient, specific heat capacity and the density of measured material.T0,tFor face temperatures, by Heater is controlled.TL,tThe temperature at end, T are placed for ultrasonic probe0For the initial temperature of test specimen.J is by transonic speed Degree is expressed as the piecewise function number with position and time change, f (Vj) it is mathematical formulae made of piecewise function fitting.
(4) heat conduction inverse problem is solved, ultrasonic propagation velocity V is obtained.
Further, matching process is as follows:
1) probe parameter of ultrasonic probe is obtained by ultrasonic probe monitoring device.
2) parameter is driven according to the probe that probe parameter obtains ultrasonic probe.
3) driving parameter ultrasonic probe is driven according to probe, matches ultrasonic probe with ultrasonic device main part.
Further, the probe parameter is the identification information of ultrasonic probe.
It is matched according to the identification information with the identification information being pre-stored in probe data library to obtain the ultrasound Corresponding probe of popping one's head in drives parameter.
Probe parameter is the identification information and probe property parameters of ultrasonic probe.
It is matched according to the identification information with the identification information being pre-stored in probe data library to obtain the ultrasound It pops one's head in corresponding probe property parameters, parameter is driven according to the probe that the probe property parameters obtain ultrasonic probe.
Further, the method for the integrated central processing element progress regulating and controlling temperature of temperature-controlling system includes:
Set a temperature threshold value of central processing element.
Judge that a maximum can handle load capacity according to temperature threshold value.
Multiple first tasks are combined into one first continuous work task according to platform power administrative skill is collected.
Judge whether a load capacity of the first continuous work task is greater than maximum and can handle load capacity.
When the load capacity of the first continuous work task, which is greater than maximum, to handle load capacity, by the first continuous work task One of overload part the first task remove the first continuous work task.
When receiving the first continuous work task, central processing element is switched into an operation mould by a suspend mode Formula, and the first continuous work task of processing.And after the completion of the processing of the first continuous work task, by central processing element It is set as suspend mode.
The operating frequency of central processing element has a normal operating frequency and method under general operation further include:
One first operating frequency is determined according to the load capacity of the first continuous work task and temperature threshold value.
And when central processing element switches to operation mode, by the operating frequency of central processing element by normally grasping Working frequency is promoted to the first operating frequency, and handles the first continuous work task by the first operating frequency.
Wherein the working frequency of the first operating frequency is higher than the working frequency of normal operating frequency.
Central processing element control method further include:
It is flat according to collecting after the processing of the first continuous work task is completed and central processing element enters suspend mode First task of multiple second tasks and part of overloading is combined into one second continuous work by platform power management techniques Make task.
When receiving the second continuous work task, central processing element is switched into operation mode by suspend mode.
The operating frequency of central processing element is promoted to one second operating frequency by normal operating frequency, passes through second Operating frequency handles the second continuous work task.And after the completion of the processing of the second continuous work task, by central processing element It is set as suspend mode.
Wherein the working frequency of the first operating frequency is higher than the working frequency of normal operating frequency.
First continuous work task is handled the time point completed and beginning using the first operating frequency by central processing element Receiving had for one first interval time between the time point of the second continuous work task, and normal frequency is used to connect first Continuous task processing, which is completed and received, had for one second interval time between the second continuous work task, wherein between first Every the time less than the second interval time.
Further, the alert device includes detector, light alarm apparatus, phonetic alarm, the detector setting In the upper end of alarm system, the light alarm apparatus is connected to the downside of detector, and the phonetic alarm is connected to light The side of line alarm.
The detection implement body is combined using sound wave detector and fixing, and sound wave detector is arranged optical fiber and leads Light unit, light element are fixed in detector body by fixing material, and fixed material is formed in around light element extremely Few a part, at least part of light element are formed by glass, and fixed material is fluorine resin material, tetrafluoroethylene-perfluoro Between dioxol polymer and fluorine silicone rubber or the refractive index low-refraction silicone resin lower than the refractive index of light element or Methyl system silicone resin, for the light exit side of light element by fixing material covering, light element includes to the light being emitted from light source The first light conducting member conducted is spread by the light of the first light conducting member conduction with making and is conducted to sound wave detector Second light conducting member, the second light conducting member light from the light incident side of the first light conducting member incidence include spreading incident light At least the second light conducting member is fixed by fixing material in light pervasion component, the first light conducting member and the second light conducting member, and first Only the second light conducting member is fixed by fixing material in light conducting member and the second light conducting member, fixing include have distal end and The long element of proximal end, fixing further include the opposed member and shell that at least one is mounted on the far-end of long element, Opposed member is arranged in a part that detector is clamped between long element and opposed member, and opposed member is from elongated structure The proximal end for being distally-oriented to long element of part extends, and opposed member is connected to long element by traversing component, traverses component quilt It is arranged as engaging the top edge of a part of detector in use, opposed member is by flexibly inclined towards long element Set, shell is mounted to long element in the side opposite with opposed member of long element, the shell by around transverse to The axis of the longitudinal direction of long element and be pivotally mounted to long element, shell is slideably pacified relative to long element Dress, the brake apparatus of the opposite sliding for preventing shell and long element, brake apparatus includes rack gear and pawl.
Further, O- methyl-isourea disulfate and oleum, concentrated nitric acid nitration reaction, obtain reaction solution.Specific packet It includes: 115% oleum being added in a kettle, cool down temperature control at -10-0 DEG C, the O- methyl-isourea sulphur being then added Sour hydrogen salt.- 10-0 DEG C of heat preservation, 98% sulfuric acid and nitric acid mixed acid is then added.Then, reaction solution is aged 24 at -5 DEG C Hour.
Further, reaction solution is added in the cooling water of temperature control, crystallization, after need to carry out:
Filter centrifugation rejection filter obtains product O- methyl N-nitro isourea.
Concentrated hydrochloric acid and methylamine water solution methylation reaction are added in O- methyl N-nitro isourea.
Sub-cooled crystallization.
Filtering, filter cake are washed with ice water.
It is dried to obtain target product O- methyl-N-methyl-N '-nitro isourea.
O- methyl-N methyl-N '-nitro isourea the production method is utilized another object of the present invention is to provide a kind of O- methyl-N methyl-N '-nitro isourea of production.
O- methyl-isourea disulfate and oleum, concentrated nitric acid occur nitration reaction and obtain O- methyl N-nitro isourea. Chemical equation are as follows:
Nitration reaction:
Methylamine reaction:
In conclusion advantages of the present invention and good effect are as follows:
By O- methyl-N methyl-N '-nitro isourea that present invention process method produces, 20% ethofenprox, dinotefuran WP 120g/hm2And 150g/hm2Processing shows good control efficiency, 1 day control efficiency to adult after medicine to rice water weevil Respectively 66.62% and 73.29%, 3,7 and 14 days preventive effects are 87.33% or more after medicine；Larva was prevented in 20 days after medicine Effect is respectively 89.62% and 92.49%, can be promoted and applied.
The present invention carries out methylation reaction at 70 DEG C, and reaction yield is high；The present invention is washed using sodium carbonate liquor It washs, the acid reactant for not participating in reaction in product can be removed, improve the precision of product, while secondary using ice water progress Washing removes the inorganic matter of all products, while reducing pollution, improves the content of product effective component, increases operation rate.
The present invention is at low cost: sulfuric acid production system is also an energy resource system, sulfate system be the present invention provide steam with Primary raw material sulfuric acid.
The present invention has oxygroup isourea disulfate production system, has raw material and transport advantage.
The a large amount of dilute sulfuric acid of by-product of the present invention, the dilute sulfuric acid of by-product can use sulfuric acid apparatus processing regeneration, it is organized and Organic gas, the sulfurous gas of uncontrollable discharge can be passed through by the sulfate system fluidized bed furnace import that negative pressure system set arrives High-temp combustion becomes water and carbon dioxide, thoroughly solves the problems, such as the smell of production, while returning rear Sulphur ressource.Dilute sulfuric acid enters sulphur It is used after acid system concentrate as sulfonation.
O- methyl-N-methyl-N '-nitro isourea produced by the invention is much smaller than demand in existing market supply, can be with Create economic value.
Cooling water of the invention is regulated and controled by temperature-controlling system, acquires ultrasonic probe using the camera of temperature-controlling system Operative scenario temperature data.Acquire ultrasonic probe temperature data in real time using temperature sensor.It is set using the measurement of temperature-controlling system Standby measurement ultrasonic propagation velocity data.Ultrasonic probe refrigeration cool-down is operated using refrigerator.Utilize automatic adaptation program pair Ultrasonic probe and ultrasonic device master unit carry out Adaptive matching operation.Using alert device according to abnormal temperature data and police Report notice.
Utilize the ultrasonic probe operative scenario temperature data information of display display acquisition.
The method that the integrated central processing element of temperature-controlling system carries out regulating and controlling temperature includes:
Set a temperature threshold value of central processing element.
Judge that a maximum can handle load capacity according to temperature threshold value.
Multiple first tasks are combined into one first continuous work task according to platform power administrative skill is collected.
Judge whether a load capacity of the first continuous work task is greater than maximum and can handle load capacity.
When the load capacity of the first continuous work task, which is greater than maximum, to handle load capacity, by the first continuous work task One of overload part the first task remove the first continuous work task.
When receiving the first continuous work task, central processing element is switched into an operation mould by a suspend mode Formula, and the first continuous work task of processing.And after the completion of the processing of the first continuous work task, by central processing element It is set as suspend mode.
The operating frequency of central processing element has a normal operating frequency and method under general operation further include:
One first operating frequency is determined according to the load capacity of the first continuous work task and temperature threshold value.
And when central processing element switches to operation mode, by the operating frequency of central processing element by normally grasping Working frequency is promoted to the first operating frequency, and handles the first continuous work task by the first operating frequency.
Wherein the working frequency of the first operating frequency is higher than the working frequency of normal operating frequency.
Central processing element control method further include:
It is flat according to collecting after the processing of the first continuous work task is completed and central processing element enters suspend mode First task of multiple second tasks and part of overloading is combined into one second continuous work by platform power management techniques Make task.
When receiving the second continuous work task, central processing element is switched into operation mode by suspend mode.
The operating frequency of central processing element is promoted to one second operating frequency by normal operating frequency, passes through second Operating frequency handles the second continuous work task.And after the completion of the processing of the second continuous work task, by central processing element It is set as suspend mode.
Warning device includes detector, light alarm apparatus, phonetic alarm, and the detector is arranged in alarm system Upper end, the light alarm apparatus is connected to the downside of detector, and the phonetic alarm is connected to light alarm apparatus Side.
Temperature control instrument of the present invention can be carried out and alarm, for production of the temperature control at positive and negative 1 degree Celsius, to production in reaction Moral character matter and purity unanimously provide guarantee.
Detailed description of the invention
Fig. 1 is the production method flow chart of O- methyl-N methyl-N '-nitro isourea provided in an embodiment of the present invention.
Fig. 2 is the production principle flow chart of O- methyl-N methyl-N '-nitro isourea provided in an embodiment of the present invention.
Fig. 3 is O provided in an embodiment of the present invention, N- dimethyl-N '-nitro isourea material balance process flow chart
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to this hair It is bright to be further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not For limiting the present invention.
Current country O- methyl-N-methyl-N '-nitro isourea production capacity much can not meet the market demand.To rice water Weevil control efficiency is poor.
To solve the above problems, the present invention is described in detail with reference to the accompanying drawing.
O- methyl-N methyl-N '-nitro isourea production method provided in an embodiment of the present invention, the O- methyl-N methyl- N '-nitro isourea production method includes: O- methyl-isourea disulfate and oleum, concentrated nitric acid nitration reaction, is reacted Liquid.Reaction solution is added in the cooling water of temperature control, crystallization.Cooling water is regulated and controled by temperature-controlling system, utilizes temperature-controlling system Camera acquires ultrasonic probe operative scenario temperature data.Acquire ultrasonic probe temperature data in real time using temperature sensor.Benefit Ultrasonic propagation velocity data are measured with the measuring device of temperature-controlling system.Ultrasonic probe refrigeration cool-down is operated using refrigerator.
Adaptive matching operation is carried out to ultrasonic probe and ultrasonic device master unit using automatic adaptation program.Utilize police Report equipment according to abnormal temperature data and alert notification.
Utilize the ultrasonic probe operative scenario temperature data information of display display acquisition.
In embodiments of the present invention, the ultrasonic velocity measurement module measurement method includes:
(1) the ultrasonic propagation velocity V under test specimen room temperature state is obtained by measuring device0。
(2) test specimen is heated, by ultrasound method, test specimen tiThe ultrasonic propagation time t at momenti,exp。
(3) Optimized model of ultrasonic propagation velocity measurement is established.The objective function of optimization are as follows:
Wherein: V is ultrasonic propagation velocity to be measured.ti,calThe t being calculated for numerical valueiThe ultrasonic wave at moment is propagated Time, the time of measuring ordinal number that subscript i is indicated, N indicate total time of measuring points.L is the length that test specimen is tested direction.
Constraint condition are as follows:
f(Vj)=V0
Wherein: k, C and ρ are respectively thermal coefficient, specific heat capacity and the density of measured material.T0,tFor face temperatures, by Heater is controlled.TL,tThe temperature at end, T are placed for ultrasonic probe0For the initial temperature of test specimen.J is by transonic speed Degree is expressed as the piecewise function number with position and time change, f (Vj) it is mathematical formulae made of piecewise function fitting.
(4) heat conduction inverse problem is solved, ultrasonic propagation velocity V is obtained.
In embodiments of the present invention, matching process is as follows:
1) probe parameter of ultrasonic probe is obtained by ultrasonic probe monitoring device.
2) parameter is driven according to the probe that probe parameter obtains ultrasonic probe.
3) driving parameter ultrasonic probe is driven according to probe, matches ultrasonic probe with ultrasonic device main part.
Further, the probe parameter is the identification information of ultrasonic probe.
It is matched according to the identification information with the identification information being pre-stored in probe data library to obtain the ultrasound Corresponding probe of popping one's head in drives parameter.
Probe parameter is the identification information and probe property parameters of ultrasonic probe.
It is matched according to the identification information with the identification information being pre-stored in probe data library to obtain the ultrasound It pops one's head in corresponding probe property parameters, parameter is driven according to the probe that the probe property parameters obtain ultrasonic probe.
In embodiments of the present invention, the method for the integrated central processing element progress regulating and controlling temperature of temperature-controlling system includes:
Set a temperature threshold value of central processing element.
Judge that a maximum can handle load capacity according to temperature threshold value.
Multiple first tasks are combined into one first continuous work task according to platform power administrative skill is collected.
Judge whether a load capacity of the first continuous work task is greater than maximum and can handle load capacity.
When the load capacity of the first continuous work task, which is greater than maximum, to handle load capacity, by the first continuous work task One of overload part the first task remove the first continuous work task.
When receiving the first continuous work task, central processing element is switched into an operation mould by a suspend mode Formula, and the first continuous work task of processing.And after the completion of the processing of the first continuous work task, by central processing element It is set as suspend mode.
The operating frequency of central processing element has a normal operating frequency and method under general operation further include:
One first operating frequency is determined according to the load capacity of the first continuous work task and temperature threshold value.
And when central processing element switches to operation mode, by the operating frequency of central processing element by normally grasping Working frequency is promoted to the first operating frequency, and handles the first continuous work task by the first operating frequency.
Wherein the working frequency of the first operating frequency is higher than the working frequency of normal operating frequency.
Central processing element control method further include:
It is flat according to collecting after the processing of the first continuous work task is completed and central processing element enters suspend mode First task of multiple second tasks and part of overloading is combined into one second continuous work by platform power management techniques Make task.
When receiving the second continuous work task, central processing element is switched into operation mode by suspend mode.
The operating frequency of central processing element is promoted to one second operating frequency by normal operating frequency, passes through second Operating frequency handles the second continuous work task.And after the completion of the processing of the second continuous work task, by central processing element It is set as suspend mode.
Wherein the working frequency of the first operating frequency is higher than the working frequency of normal operating frequency.
First continuous work task is handled the time point completed and beginning using the first operating frequency by central processing element Receiving had for one first interval time between the time point of the second continuous work task, and normal frequency is used to connect first Continuous task processing, which is completed and received, had for one second interval time between the second continuous work task, wherein between first Every the time less than the second interval time.
In embodiments of the present invention, the alert device includes detector, light alarm apparatus, phonetic alarm, described The upper end of alarm system is arranged in detector, and the light alarm apparatus is connected to the downside of detector, the audio alert Device is connected to the side of light alarm apparatus.
The detection implement body is combined using sound wave detector and fixing, and sound wave detector is arranged optical fiber and leads Light unit, light element are fixed in detector body by fixing material, and fixed material is formed in around light element extremely Few a part, at least part of light element are formed by glass, and fixed material is fluorine resin material, tetrafluoroethylene-perfluoro Between dioxol polymer and fluorine silicone rubber or the refractive index low-refraction silicone resin lower than the refractive index of light element or Methyl system silicone resin, for the light exit side of light element by fixing material covering, light element includes to the light being emitted from light source The first light conducting member conducted is spread by the light of the first light conducting member conduction with making and is conducted to sound wave detector Second light conducting member, the second light conducting member light from the light incident side of the first light conducting member incidence include spreading incident light At least the second light conducting member is fixed by fixing material in light pervasion component, the first light conducting member and the second light conducting member, and first Only the second light conducting member is fixed by fixing material in light conducting member and the second light conducting member, fixing include have distal end and The long element of proximal end, fixing further include the opposed member and shell that at least one is mounted on the far-end of long element, Opposed member is arranged in a part that detector is clamped between long element and opposed member, and opposed member is from elongated structure The proximal end for being distally-oriented to long element of part extends, and opposed member is connected to long element by traversing component, traverses component quilt It is arranged as engaging the top edge of a part of detector in use, opposed member is by flexibly inclined towards long element Set, shell is mounted to long element in the side opposite with opposed member of long element, the shell by around transverse to The axis of the longitudinal direction of long element and be pivotally mounted to long element, shell is slideably pacified relative to long element Dress, the brake apparatus of the opposite sliding for preventing shell and long element, brake apparatus includes rack gear and pawl.
The invention will be further described combined with specific embodiments below.
Embodiment
As shown in Figure 1-3, the production method packet of O- methyl-N methyl-N '-nitro isourea provided in an embodiment of the present invention It includes:
115% oleum is added into clean, anhydrous reaction kettle by S101, and cooling temperature control is at -10-0 DEG C, then It is slowly added to O- methyl-isourea disulfate.After keeping the temperature at -10-0 DEG C of a period of times, be then added 98% sulfuric acid and Nitrate mixture carries out nitration reaction, obtains reaction solution, reaction solution is aged 24 hours at -5 DEG C.
Tap water is added into refining kettle by S102, and cooling 2 DEG C of temperature control into refining kettle hereinafter, be slowly added to while stirring Reaction solution after ageing, and continue to be aged 3 hours progress crystallizations at -10 DEG C.
S103, centrifugal rejection filter obtains O- methyl N-nitro isourea after filtering.
S104: O- methyl N-nitro isourea, 36% concentrated hydrochloric acid, 40% methylamine water of content 85% are added into reaction kettle Temperature is risen to 70 DEG C of 4-6 hours of progress methylation reaction while stirring by solution.
S105: after complete reaction, being cooled to 0-2 DEG C with ice water, and crystallizes 2 hours at a temperature of this.
S106: filtering, filter cake are first washed 2-3 times with sodium carbonate liquor, are then washed 1-2 times again using ice water.
S107: it is filtered dry, is dried to obtain target product O- methyl-N-methyl-N '-nitro isourea.
Nitration reaction chemical equation provided in an embodiment of the present invention are as follows:
Methylamine reaction provided in an embodiment of the present invention:
Application principle of the invention is further described combined with specific embodiments below.
Embodiment:
1) capital equipment
2) technical process
Ensure the clean foreign of reaction kettle, 115% oleum 450kg is added in no moisture in 3000L reaction kettle, cold But then temperature control is slowly added into O- methyl-isourea disulfate 450kg obtained above at -10-0 DEG C.- 10-0 DEG C of heat preservation, so Nitration mixture 920kg (98% sulfuric acid 650kg and nitrate mixture 270kg) is added afterwards.Then, reaction solution is aged 24 at -5 DEG C Hour.
Water 1980kg is added in 5000L refining kettle, cooling 2 DEG C of temperature control into refining kettle hereinafter, be slowly added into above-mentioned old Reaction solution after change.After the solution is aged 3 hours at -10 DEG C, centrifugal rejection filter obtains product O- methyl-N- nitre after filtering Base isourea 300kg.
Be added in 3000L reaction kettle the O- methyl N-nitro isourea of 600kg content 85%, 36% concentrated hydrochloric acid 870kg, Temperature is risen to 70 DEG C of 4-6 hours of progress methylation reaction while stirring by 40% methylamine water solution 664kg.Fully reacting Afterwards, ice water is cooled to 0-2 DEG C, crystallizes 2 hours, then filters, filter cake is first washed 2-3 times with sodium carbonate liquor, so in this temperature It is washed 1-2 times again using ice water afterwards, is filtered dry, is dried to obtain O- methyl-N-methyl-N '-nitro isourea of 486kg.
3) technical standard and technical indicator
Product technology standard is referring to following standard:
A) GB/T 601-2002 chemical reagent preparations of standard volumetric solutions.
B) preparation of GB/T 602-2002 chemical reagent impurity determination standard solution.
C) in GB/T 603-2002 chemical reagent test method preparation and product used preparation.
D) GB/T 9729-2007 chemical reagent chloride determination universal method.
E) universal method 1 of the industrial chemical products iron content measurement of GB/T 3049-2006,10- ferrosin are divided light Degree method.
F) GB/T 6682-2008 water for analytical laboratory use-Specification and test methods.
G) GB/T 6678-2003 chemical products sample general provisions.
H) GB/T 8170-2008 rules of rounding off for numerical values & expression and judgement of limiting values.
Technical indicator
1 O- methyl-N methyl-N ' of table-nitro isourea product specification and quality index
4) result
Certain province Agricultural Environmental Monitoring station, academy of agricultural sciences's plant protection analysis institute the result shows that, 20% ethofenprox, dinotefuran WP 120g/hm2And 150g/hm2Processing shows good control efficiency, 1 day control efficiency to adult after medicine to rice water weevil Respectively 66.62% and 73.29%, 3,7 and 14 days preventive effects are 87.33% or more after medicine.Larva was prevented in 20 days after medicine Effect is respectively 89.62% and 92.49%, can be promoted and applied.
Rice black-tailed leafhopper.By field trial, dinotefuran etc. is several new for Agro-ecology and plant protection management master station Control efficiency of the medicament to rice field rice green leafhopper.The results show that 20% dinotefuran WG 300-450 g/hm2,30% Nitenpyram WG 300g/hm2,50% pymetrozine 150g/hm2+20% dinotefuran WG, 300 g/hm2 to the control efficiency of rice green leafhopper compared with Good, 15-28 days after medicine, Rectifying efficacies reach 94.54%-100%.
Rice ragged stunt virus.It is 0.06% dinotefuran SP of analysis that Shanghai Pudong New District Agriculture Technology Promotion Center, which analyzes personnel, To the control efficiency of Rice ragged stunt virus, optimal dose and safety etc., for the pesticide large scale application provide science according to According to spy has carried out related pharmacodynamic test.The result shows that 0.06% dinotefuran SP is significant to Rice ragged stunt virus control efficiency, and to water Rice growth safety.It is recommended that 3-5 days before rice cut, pink rice borer egg hatching peak medication, 0.06% dinotefuran SP of every 667m2 15-20kg can obtain ideal control efficiency.
Small wheat midge.Institute, Henan Province Weihui City agricultural technology extension center analysis people are analyzed in academy of agricultural sciences's plant protection Member prevents and treats wheat midge with 20% dinotefuran SG of various dose is spraying in wheat full heading time, the results showed that, 20% To the control efficiency of wheat midge up to 90% or more when dinotefuran SG dosage is 20,25 and 30g/667m2.
Radish striped flea-beetle.Plant protection master station, Hubei biotechnology Professional School analysis 20% dinotefuran SC of personnel are anti- Radish striped flea-beetle field control effectiveness test result is controlled to show in striped flea-beetle adult initial phase, with 20% dinotefuran SC 20mL, 30mL, 40mL/667m2 dosage spray are prevented and treated, and 3 days average preventive effects are 71.77%, 73.16% and 74.71% after medicine, with life The preventive effect that 45% chlopyrifos EC 50mL/667m2 of medicament is commonly used in production is suitable, after application 7 days preventive effects be respectively 84.49%, 85.69% and 86.25%.15 days preventive effects are respectively 75.68%, 77.15% and 78.07% after medicine, are significantly higher than 45% poison Dead tick EC 50mL/667m2.Consider from production, it is proposed that use 20% dinotefuran SC 20mL-40mL/667m2, spray value 45L-50 L/667m2 is advisable.
Academy of agricultural sciences vegetables analyse the dinotefuran suspending agent that analyzed personnel carry out scientifically and prevent and treat radish phyllotreta striolata drug effect Test result shows that dinotefuran prevents and treats phyllotreta striolata with good under the conditions of 120g/hm2,90g/hm2,60g/hm2 Control efficiency, 3 days preventive effects are respectively 99.32%, 96.97%, 93.61% after medicine, and have preferable quick-acting, lasting period It is 7 days or so.It is recommended that carrying out wheel use with other pesticides.
Tomato Bemisia tabaci.Plant protection station analysis personnel analyze several medicaments to the control efficiency of tomato Bemisia tabaci, knot Fruit shows that+22.4% spiral shell worm second rouge 1000 times of liquid buckets of suspending agent of SG1000 times of liquid of 20% dinotefuran mix medicament to Bemisia tabaci adults There is preferable control efficiency with nymph, the control efficiency of 7 days adults and nymph is respectively 88.40%, 76.30% after medicine.It builds View mixes technology using two kinds of medicament barrels of dinotefuran and spiral shell worm second rouge when preventing and treating tomato Bemisia tabaci.
Sugarcane moth borer, thrips and woolly aphid.Plant quarantine station, the inspection of the Ministry of Agriculture, Jilin Agriculture University ginseng and pilose antler product quality supervision Test center, Guangxi Tianyuan Biochemical Co., Ltd. analysis personnel are tested to 0.05% dinotefuran medicament-fertilizer mixture prevention and treatment sugarcane evil Worm is analyzed, the results show that 0.05% dinotefuran medicament-fertilizer mixture has preferable prevention and treatment effect to sugarcane moth borer and thrips Fruit exists between dosage and preventive effect and is positively correlated, i.e., preventive effect is improved with the increase of dosage, and product recommends dosage: 300- 400kg/hm2。
Academy of agricultural sciences's plant protection analyze analyze personnel analyze the result shows that, when sugarcane is sowed, per hectare applies 20% SG180-240 grams of dinotefuran, 100% is reached as high as to the preventive effect of seedling stage sugarcane moth borer, to the preventive effect of sugar cane cottony aphid up to 95% More than, and the lasting period is long, and the preventive effect with 25% Diacloden WG is prevent and treat sugarcane moth borer and woolly aphid efficient low without significant difference The favourable agents of poison.
Cowpea trialeurodes vaporariorum.Nanchong City plant test station for plant protection, plant test station for plant protection analyze personnel's cowpea Trialeurodes vaporariorum Westwood pesticide field Pharmacodynamic test the result shows that, in the case where heavier situation occurs for greenhouse autumn cowpea trialeurodes vaporariorum, 1.8% Avermectin of per hectare Plain EC 375g, 20% dinotefuran SP 600g, 5% Acetamiprid WP 600g, 25% pymetrozine WP 600g (comparison medicament), 5-8 Its application 1 time, continuous administration 3 times, 7 after medicine, 14,20 days, control efficiency respectively up to 90.9%, 97.0%, 88.0%, 93.9%, 97.4%, 92.1%, 84.2%, 89.4% and 95.6%, 86.7%, 82.2%, 84.5%, and 7 days furans after medicine Worm amine and avermectin and pymetrozine, extremely significant to be higher than Acetamiprid, difference is not shown between avermectin and Acetamiprid and pymetrozine It writes；14 days after medicine, avermectin and dinotefuran and pymetrozine difference be not significant, extremely significant to be higher than Acetamiprid, dinotefuran and pyrrole Aphid ketone difference is not significant, is significantly higher than Acetamiprid；20 days after medicine, avermectin is extremely significant to be higher than dinotefuran, Acetamiprid and pyrrole aphid Ketone, dinotefuran and Acetamiprid and pymetrozine difference be not significant.Meanwhile biological pesticide avermectin, 7 days after medicine, preventive effect is slightly lower 14 days after chemical pesticide dinotefuran, medicine, preventive effect is higher than dinotefuran, and 20 days after medicine, preventive effect is extremely significant to be higher than dinotefuran.Think This 4 kinds of medicaments especially biological pesticide avermectin acts not only as the favourable agents of prevention and treatment Trialeurodes vaporariorum Westwood, and can be with Favourable agents as modern agriculture demonstration area, non-polluted farm product, green agricultural product and organic farm products.
Eriosoma lanigerum.It is prevention and treatment of the clearly hidden medication to eriosoma lanigerum that analyzed personnel are analyzed in academy of agricultural sciences's plant protection Effect determines 25% Diacloden SC, 50% pymetrozine WP, 40% dinotefuran SP, 24% using " trunk winds strap method " Control efficiency of the sulfoxaflor SC to eriosoma lanigerum.The result shows that 25% Diacloden SC 100-200 times dilution, 50% Pymetrozine WP 50-100 times dilution, 40% dinotefuran SP 50-100 times dilution, 24% sulfoxaflor SC 50-100 times Dilution is 84.94%-89.28% to the control efficiency of eriosoma lanigerum.It is recommended that being promoted and applied in production.
Papillosa.Academy of agricultural sciences's plant protection analyzes analyzed personnel using conventional spray-on process, compares several medicaments pair The indoor virulence and field efficacy of Papillosa nymph.The Toxicity Determination result shows have 5 kinds of medicament virulence higher, successively Are as follows: carbosulfan > gamma cyhalothrin > Acetamiprid > metrifonate > dinotefuran, 24 hours LC50 are respectively 4.24, 6.43,7.57,11.55,14.14mg/L.Table of field test results are bright, 5% gamma cyhalothrin EW, 20% dinotefuran SG, If after 25% Acetamiprid EC, 200g/L carbosulfan EC, 90% metrifonate crystal, 1000 times of liquid medicines 1-14 days to Papillosa The preventive effect of worm be respectively 99.26%-100%, 91.77%-100%, 80.40%-90.09%, 78.37%-85.65%, 80.33%-91.14%.5% gamma cyhalothrin EW and 20% dinotefuran SG to the control efficiency of Papillosa nymph most Good, the preventive effect of 25% Acetamiprid EC and 90% metrifonate crystal is general, and the preventive effect of 200g/L carbosulfan EC is then opposite It is poor.
Small brown rice planthopper.Planting industry center analysis personnel in farm analyze several medicaments to small brown rice planthopper using field plot trial method Control efficiency and application security.Test result shows 50% sulfoxaflor WG 300g/hm2,25% Diacloden WP 120g/hm2 and 25% dinotefuran WP 240g/hm2 has preferable quick-acting, high efficiency and lasting effect, and safety is good, it is proposed that It is promoted and applied in production.Cotton plant bug
Agrotechnical master station, institute of agricultural sciences analysis personnel are clear control efficiency of the 20% dinotefuran SG in cotton field to fleahopper silk worm, Carry out field control effectiveness test within 2011 and 2012, the results showed that, 1 after medicine, 3,5,7 days, 20% dinotefuran SG 60- 120g/hm2 is respectively 53.04%-71.94%, 61.45%-81.15%, 71.91%- to the preventive effect of cotton plant bug silk worm 86.34% and 81.87%-92.80% has preferable control efficiency, and to cotton safety.
Academy of agricultural sciences cotton analysis institute analysis personnel analyze 6 kinds of insecticides to the field control effect of cotton plant bug.As a result table Bright, 50% sulfoxaflor WG is rich according to 60g/hm2 and 40% rice according to 75g/hm2 (effective component), 20% dinotefuran SG Dissipate, after Lambda-Cyhalothrin is according to 450g/hm2 use, integrated control effect is preferable, and not only quick-acting is fast, but also the lasting period compared with It is long, it is better than 97% orthene WG of common insecticide, 45% malathion EC and 2.5% Lambda-Cyhalothrin.Due to 50% sulfoxaflor WG, 20% dinotefuran SG and 40% phenthoate dimephenthoate cidial, Lambda-Cyhalothrin all have high-efficiency low-toxicity safety The features such as, effect on environment is small, it is proposed that the favourable agents as integrated control cotton plant bug.
Below with reference to effect, the invention will be further described.
Design for Automatic Control Engineering of the present invention is technologically advanced, safe and reliable, easy to operate and economical rationality principle carries out, and is saving Under the premise of investment, whole process automatization level is improved, to improve the yield and quality of product, while mitigating operator's Labor intensity.Important technological parameter leads to control room and carries out centralized displaying, record, alarm and control.Control room instrument uses Conventional simulation instrument (based on read out instrument), recording apparatus select recording instrument without paper.The prison of general technology procedure parameter Control is based on on-the-spot make an inspection tour, operation.To guarantee total system safe operation, the present invention is provided with perfect automatic control system, right Production process carries out necessary monitoring and interlocked control, once occur cutting off the water supply, the abnormal phenomenon such as fracture when, system issues report Alert signal or interlocked control relevant device are out of service.
The present invention, for principle, according to the significance level of process in production, stresses to consider automatic control with simple, practical and reliable It is operated with optimization, design executes HG20505-HG20516 (92) standard and existing other standards, and measurement unit uses SI unit System.
Instrument selected by the present invention and control equipment are advanced, reliable, it is ensured that long-term, the safety of process unit Production and operation.In conjunction with the practical experience that domestic chemical industry instrument uses, instrument selection is with technologically advanced, safe and reliable, dimension Shield is convenient and economical rationality is principle.Based on domestic imported technology co-production, the more successful instrument of scene use.It is outdoor The instrument of installation meets round-the-clock requirement, and degree of protection is not less than IP55 in principle, and the occasion of special requirement adds instrument protection Case is protected.
Online temperature measurement, selects corrosion-resistant thermometer；Online pressure measurement selects spring manometer and diaphragm type resistance to Lose pressure gauge；Water meter and spinner flowmeter and anti-corrosion electric magnetic flowmeter are selected in online flow measurement；The measurement of teletransmission temperature, choosing With Pt100 thermal resistance thermometer, K-type thermal resistance thermometer and radiation high-temperature thermometer, secondary meter is cooperated to carry out display note Record.Remote liquid level measurement, selects fluid level transmitter and differential pressure transmitter, and cooperation instrument is shown.Whirlpool is selected in teletransmission flow measurement Street flowmeter and electromagnetic flowmeter, cooperation secondary meter are shown.Repairing instrument: in addition to light maintenance adjustment, other are mentioned by supplier For.
Process of the present invention monitoring and measuring is controlled using domestic advanced special instrument, instrument at present.DCS system More professional computer control system is selected, technique is carried out automatically controlling, it is ensured that process monitoring and measurement are accurate, controllable.
The present invention uses domestic and international advanced technologies power-saving technology, domestic advanced energy-efficient equipment is selected, using continuous Production method, scale device, and designed using Fieldbus Control, guarantee runs smoothly reliable；Height automation reaches employment Less, purpose high-efficient, product quality is high and energy-saving effect is good.
The present invention selects advanced energy-efficient equipment, and blower fan of cooling tower is using the blower that performance is good, air quantity is big, high-efficient. Water pump is all made of the higher water pump of slow-speed of revolution efficiency, the water supply system that water consumption changes greatly, using frequency conversion equipment.Life water Pressurizing device makes full use of garden municipal water supply ductwork pressure using no negative pressure automatic frequency-conversion water supply device.
Residual heat resources of the present invention recycle, and distillation process absorbs the condensation heat reuse of tower top using water.It selects and efficiently protects Adiabator heat exchanging equipment, high/low temperature pipeline are kept the temperature, and heat preservation, insulating layer thickness are meteorological by relative national standards and locality Condition reduces heat loss, reduces energy consumption by determining after calculating.
Electric system energy conservation measure of the present invention:
(1) electric substation is located at load concentration, the biggish place of single motor capacity when environment allows；
(2) electrostatic condenser is arranged in electric substation to compensate, improves power factor (PF)；
(3) Transformer Selection low-loss energy-saving type；
(4) converter plant can be used to save electric energy in the pump of process requirement gearshift adjustment；
(5) lighting source is selected energy-saving, such as power saving fluorescent lamp, Metal halogen lamp；
(6) high-tension cable of high current checks its cable core cross-section by economic current density.
Heat preservation energy-saving of the present invention, in the place of the needs such as equipment pipe heat preservation, using the higher thermal insulating material of the ratio of performance to price Material reaches preferable energy-saving effect, and 350 DEG C or more are kept the temperature using microporous calcium silicate, outsourcing galvanized iron sheet, 350 DEG C or less uses Rock wool or perlite products heat preservation, outsourcing galvanized iron sheet reduce radiation loss to the greatest extent.
Control system of the present invention uses advanced distributing (DCS) control system, by computer controlled machine group start and stop, Data processing and parameter adjustment are carried out, and provides unit operation information to operations staff in time, when any abnormal work occurs for unit When condition, alarm is issued in time, realizes unit safety economical operation.It is further perfect in order to reinforce operational management and business accounting The metering and monitoring device of each process system, have all installed sufficient amount of metering or measuring instrument on various process systems, Especially measuring instrument is equipped with external associated vapour, water, electricity etc..
The present invention selects energy-saving equipment product, and various electrical equipments select energy-conserving product, use variable-frequency motor, transformation The low-pressure side of device fills power capacitor compensating power, to improve the power factor of power supply system, reduces reactive loss.
The present invention presses energy saving principle for service cable in energy-saving electricity and distribution line and selects conductor cross-section；Distribution design Make distribution facility close to the biggish equipment of load as far as possible；Lighting source uses Novel energy-saving lamp, is meeting device illumination and light Under conditions of color, lamps and lanterns dosage and lamps and lanterns capacity are reduced, energy saving purpose is reached
Energy-efficient sophisticated equipment is used in energy-saving effect of the present invention, and takes comprehensive effective section in the design Measure can and be measured, consumption index is enabled the invention to and is substantially better than professional standard, energy-saving effect is obvious.
The warm water discharge of cooling equipment is reused after cooling tower cooler in water saving measures of the present invention, and system only needs to mend Fill the water of the losses such as evaporation, leakage, blowdown.By following measures in circulation, water-saving purpose can reach.It is appropriate to add The concentration rate (taking 2.5) of systemic circulation cooling water, to reduce the water amount of blowdown of cooling tower；It is arranged in cooling tower and efficiently removes Hydrophone, to reduce its wind water loss；Regulating valve is set on water supply pipe, to control overflow water loss.
(1) all condensed waters are collected；
(2) circulation increases anti-incrustation corrosion inhibitor, improves cycles of concentration, reduces blowdown and amount of makeup water；
(3) cooling water employed in entire project is all made of recirculated water to save water resource；
(4) circulating water cooling tower uses advanced water collection device, can reduce windage loss；
(5) recirculated water concentration rate is greater than 3, can reduce amount of makeup water；
(6) metering regulating system respectively is installed with water spot, flow control is carried out to watering equipment.
The calculating principle of energy-saving and emission-reduction amount of the present invention:
(1) electricity of the energy-saving technological measures saving such as converter technique is utilized.
(2) emission reduction total amount implements the total amount that harmful substance contents in the sewage of front and back calculate emission reduction sewage by detection.
(3) energy-saving and emission-reduction amount is only limitted to after optimizing technique by implementing energy-saving and emission-reduction of the present invention, reduced energy consumption with " three wastes " total amount of emission reduction.
Below with reference to Wastewater Pollutant generation link and pollution prevention measure, the invention will be further described.
(1) nitration mixture that the centrifuge separation of O- methyl N-nitro isourea generates
O- Methyl Isourea Sulfate passes through digestion, crystallization, is centrifugally separating to obtain O- methyl N-nitro isourea, and centrifugation generates Nitration mixture the further collection material of mother liquor subsider is squeezed by submerged pump after, squeeze into 100 cubes of spent acid pond, nitration mixture is mainly Sulfuric acid, concentration is between 40-45%, a small amount of O- methyl N-nitro isourea and O- Methyl Isourea Sulfate.Nitration mixture uses Sulfate system Pintsch process processing, Pintsch gas by sulfuric acid purification system, drying system, into conversion system again The concentrated sulfuric acid is prepared, decomposes carbon dioxide and nitrogen under organic matter high temperature aerobic environment.
(2) O- methyl-N-methyl-N '-nitro isourea centrifuge mother liquor is separated:
O- methyl N-nitro isourea is reacted with methylamine water solution, is centrifugated product O- methyl-N-methyl-N '-nitro After isourea, be centrifuged generation filtrate the further collection material of mother liquor subsider is squeezed by submerged pump after, filtrate be added sodium hydroxide The methylamine in filtrate is travelled out, desorption tower used, excessive methylamine in de- analysis reaction, the methylamine gas of de- analysis are then entered at 60 DEG C The methylamine hydrochloride salting liquid for being configured to 30-40% is collected in condensation, and gas reusing dilute hydrochloric acid absorbs after condensation, and gas uses level-one It is discharged after falling film absorption+second level packing material absorbing processing through 15m maximum discharge cylinder.Methylamine hydrochloride salting liquid is used as methylamine reaction Raw material.Liquid after removing methylamine is through active carbon adsorption organic matter, and then evaporative crystallization recycles sodium chloride, and evaporation condensed water is used In nitration reaction water supplement.
Exhaust gas pollution node of the present invention and prevention and cure of pollution are arranged:
(1) nitrification generates exhaust gas
It is added dropwise during oleum in nitrifying process, a small amount of NO2 and SO3 (in terms of sulfuric acid and nitric acid mist) tail gas are used It is incorporated to the exhaust treatment system of sulfate system after 98% sulfuric acid absorption, is discharged through exhaust tube.Absorption efficiency is up to 99.9%, at year The reason time is 7200h, and the concentrated sulfuric acid after absorbing acid mist is used for nitration reaction.
(2) O- methyl-N-methyl-N '-nitro isourea dry waste gas
O- methyl-N-methyl-N '-nitro isourea dry waste gas main component is methylamine and water, and dry gas is inhaled with water It receives, absorbing liquid is incorporated to the methylamine hydrochloride solution recycling of front.Absorbing liquid is water, and absorption efficiency reaches one up to 99% Determine the methylamine hydrochloride solution for being incorporated to front after concentration, utilized in methylamine workshop section, handling the time year is 7200h.
Wastewater Pollutant discharge of the present invention, waste water carry out shunting of removing contamination, i.e., peace and quiet waste water is by always arranging a mouthful direct emission.It is raw After production method waste water O- methyl-N-methyl-N '-nitro isourea sewage-treatment plant is handled respectively, it is back to production, not outlet. Outlet after sanitary wastewater is handled by company's sewage plant.
The pollution control measures of non-normal emission of the present invention:
The present invention can generate fire-fighting waste water when fire, which occurs, for device to carry out fire-fighting.Fire-fighting waste water assume office thus size, Material leakage amount difference, water and contained pollutant component and concentration are also different, change complex.By this part, water is gathered up After coming, then gradually sewage-treatment plant is sent to be handled.In conjunction with light electrolysis and Fenton reagent (iron filings, carbon and hydrogen peroxide combination) Method, generates " primary battery " effect first between iron carbon, and current potential does electrolyte up to 1.2v, primary battery with sewage, passes through Electric discharge carries out electrolytic oxidation to sewage and closes reduction treatment, newly generates [OH], [H] (reducibility coenzyme), [O] in treatment process With many components in sewage redox reaction can occur for (oxidisability coenzyme), Fe2+, Fe3+, reach degradation organic contamination The mesh of object.In addition, Fe2+ and hydrogen peroxide that electrolysis is formed are combined into Fenton reagent, oxidisability is very strong, can destroy organic Chromophoric group, auxochrome group and chain rupture in substance reach degradation and decolorization effect.(3) sewage of light electrolysis degradation and decolorization passes through It neutralizes, flocculation sedimentation；(4) using dilution appropriate, the content of chloride ion and salinity is reduced, makes chloride ion lower than 0.5%, Then in conjunction with Anaerobic Treatment (processing small-molecule substance) and aerobic degradation.(5) last sewage uses chlorbenside bacterium.
Discussion On Ecological Environment Protection Measures of the present invention:
1) clean preparation method is used, disposal of pollutants is controlled from source.Reinforce construction and the pipe of pollution prevention measure Reason controls influence of the disposal of pollutants to periphery ecological environment.
The present invention opens as far as possible to being possible to generate the station of the equipment, pipeline revealed in the case where meeting process conditions Open arrangement.Necessary sealing device or washing system are considered from technological design to the unit for being possible to evolution pernicious gas System, centralized processing are discharged into atmosphere after reaching the standard for meeting country.To prevent process units from generating toxic, nuisance accumulation, The ventilating system of reliable design.Harm of the pernicious gas to human body in order to prevent should take measures to prevent this kind of gas from escaping, Negative-pressure operation is used as far as possible, it, should also be into addition to carrying out narrow examination to weld seam for equipment and pipeline with press operation Row hydraulic pressure and air-tight test.Analysis is also easy to produce toxic gas position, vent cabinet is arranged, to ensure good operating environment.
The present invention generates 40% Waste Sulfuric Acid, can use the Waste Sulfuric Acid of fluidized bed furnace processing 40%.Postpartum profit of the invention Up to height, ratio for input and output is high.
At present product of the present invention cost of material 5.3 ten thousand or so (two tons 3.8 ten thousand yuan of hydrogen salt, 0.63 ton 0.8 ten thousand of methylamine, His raw material hydrochloric acid, sodium chloride are 7000 yuan total), 10,000 yuan/ton of three-protection design cost, 13.6 ten thousand yuan/ton of market price.Zhejiang is prompt Current 13.6 ten thousand yuan/ton of price up to Lianyun Harbour Xin Furong Science and Technology Ltd., Acquisition Company, Science and Technology Ltd., cost is 9.5 Ten thousand/ton, Qing Jiang chemical industry Huang gang, Wuhan company build up rear price and expect to drop to 130,000 yuan/ton, and cost is estimated in 8.5 ten thousand/ton. Existing market is high close to 180,000/ton, and due to being that fixed point is processed, price comparability is poor.
The present invention, which produces dilute sulfuric acid used, to be used to concentrate by recycling and reusing and produce the concentrated sulfuric acid, sulfuric acid is greatly decreased and is disappeared The cost of disposal of consumption and the three wastes；Waste water adds the technique of extraction to recycle organic phase to greatest extent using resin, reduces product The unit consumption of primary raw material.
Product of the present invention domestic production producer is less, the huge market demand, city with good economic efficiency and wide Field prospect；The infrastructure such as present invention water supply, sewage plant, sewage network, central heating, power supply are perfect；Exhaust gas, is consolidated waste water Useless, noise can qualified discharge after administering.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.

Claims (9)

1. a kind of O- methyl-N methyl-N '-nitro isourea production method, which is characterized in that the O- methyl-N methyl-N '-nitre Base isourea production method includes: O- methyl-isourea disulfate and oleum, concentrated nitric acid nitration reaction, obtains reaction solution；It will Reaction solution is added in the cooling water of temperature control, crystallization；Cooling water is regulated and controled by temperature-controlling system, utilizes the camera of temperature-controlling system Acquire ultrasonic probe operative scenario temperature data；Acquire ultrasonic probe temperature data in real time using temperature sensor；Utilize temperature control The measuring device of system measures ultrasonic propagation velocity data；Ultrasonic probe refrigeration cool-down is operated using refrigerator；
Adaptive matching operation is carried out to ultrasonic probe and ultrasonic device master unit using automatic adaptation program；Utilize alert device According to abnormal temperature data and alert notification；
Utilize the ultrasonic probe operative scenario temperature data information of display display acquisition.
2. O- methyl-N methyl-N '-nitro isourea production method as described in claim 1, which is characterized in that the ultrasonic velocity Measurement module measurement method includes:
(1) ultrasonic propagation velocity under test specimen room temperature state is obtained by measuring device；
(2) test specimen is heated, by ultrasound method, test specimen tiThe ultrasonic propagation time t at momenti,exp；
(3) Optimized model of ultrasonic propagation velocity measurement is established；
(4) heat conduction inverse problem is solved, ultrasonic propagation velocity is obtained.
3. O- methyl-N methyl-N '-nitro isourea production method as described in claim 1, which is characterized in that matching process is such as Under:
1) probe parameter of ultrasonic probe is obtained by ultrasonic probe monitoring device；
2) parameter is driven according to the probe that probe parameter obtains ultrasonic probe；
3) driving parameter ultrasonic probe is driven according to probe, matches ultrasonic probe with ultrasonic device main part.
4. O- methyl-N methyl-N '-nitro isourea production method as claimed in claim 3, which is characterized in that the probe parameter For the identification information of ultrasonic probe；
It is matched according to the identification information with the identification information being pre-stored in probe data library to obtain the ultrasonic probe Corresponding probe drives parameter；
Probe parameter is the identification information and probe property parameters of ultrasonic probe；
It is matched according to the identification information with the identification information being pre-stored in probe data library to obtain the ultrasonic probe Corresponding probe property parameters drive parameter according to the probe that the probe property parameters obtain ultrasonic probe.
5. O- methyl-N methyl-N '-nitro isourea production method as described in claim 1, which is characterized in that temperature-controlling system is integrated Central processing element carry out regulating and controlling temperature method include:
Set a temperature threshold value of central processing element；
Judge that a maximum can handle load capacity according to temperature threshold value；
Multiple first tasks are combined into one first continuous work task according to platform power administrative skill is collected；
Judge whether a load capacity of the first continuous work task is greater than maximum and can handle load capacity；
When the load capacity of the first continuous work task, which is greater than maximum, to handle load capacity, by one of first continuous work task First task of overload part removes the first continuous work task；
When receiving the first continuous work task, central processing element is switched into an operation mode by a suspend mode, with And the first continuous work task of processing；And after the completion of the processing of the first continuous work task, central processing element is set as stopping Sleep mode；
The operating frequency of central processing element has a normal operating frequency and method under general operation further include:
One first operating frequency is determined according to the load capacity of the first continuous work task and temperature threshold value；
And when central processing element switches to operation mode, by the operating frequency of central processing element by normal operating frequency It is promoted to the first operating frequency, and the first continuous work task is handled by the first operating frequency；
Wherein the working frequency of the first operating frequency is higher than the working frequency of normal operating frequency；
Central processing element control method further include:
After the processing of the first continuous work task is completed and central processing element enters suspend mode, according to collecting platform power First task of multiple second tasks and part of overloading is combined into one second continuous work task by administrative skill；
When receiving the second continuous work task, central processing element is switched into operation mode by suspend mode；
The operating frequency of central processing element is promoted to one second operating frequency by normal operating frequency, passes through the second operation frequency Rate handles the second continuous work task；And after the completion of the processing of the second continuous work task, central processing element is set as stopping Sleep mode；
Wherein the working frequency of the first operating frequency is higher than the working frequency of normal operating frequency；
First continuous work task is handled the time point completed and starts to receive by central processing element using the first operating frequency To having for one first interval time between the time point of the second continuous work task, and use normal frequency by the first continuous work Task processing, which is completed and received, had for one second interval time between the second continuous work task, wherein the first interval time is small In the second interval time.
6. O- methyl-N methyl-N '-nitro isourea production method as described in claim 1, which is characterized in that the warning device Including detector, light alarm apparatus, phonetic alarm, the upper end of alarm system, the light is arranged in the detector Alarm is connected to the downside of detector, and the phonetic alarm is connected to the side of light alarm apparatus；
The detection implement body is combined using sound wave detector and fixing, and optical fiber and leaded light list is arranged in sound wave detector Member, light element are fixed in detector body by fixing material, and fixed material is formed at least one around light element At least part of part, light element is formed by glass, and fixed material is two between fluorine resin material, tetrafluoroethylene-perfluoro Oxygen cycloolefine polymer and fluorine silicone rubber or the refractive index low-refraction silicone resin or methyl lower than the refractive index of light element It is silicone resin, the light exit side of light element includes carrying out to the light being emitted from light source by fixing material covering, light element Conduction the first light conducting member and make by the first light conducting member conduct light spread and conduct to sound wave detector second Light conducting member, the second light conducting member include that the light for spreading incident light is spread from the light incident side of the first light conducting member incidence in light At least the second light conducting member is fixed by fixing material in component, the first light conducting member and the second light conducting member, the first light conducting member With only the second light conducting member is fixed by fixing material in the second light conducting member, fixing includes elongated with proximally and distally Component, fixing further include the opposed member and shell that at least one is mounted on the far-end of long element, opposed member quilt It is arranged as clamping a part of detector between long element and opposed member, opposed member is distally-oriented to from long element The proximal end of long element extends, and opposed member is connected to long element by traversing component, traverses component and be arranged in use The top edge of a part of middle engagement detector, opposed member are resiliently biased towards long element, and shell is elongated The side opposite with opposed member of component is mounted to long element, and the shell is by around transverse to the longitudinal direction of long element The axis in direction and be pivotally mounted to long element, shell is slidably mounted relative to long element, for preventing shell The brake apparatus of opposite sliding with long element, brake apparatus includes rack gear and pawl.
7. O- methyl-N methyl-N '-nitro isourea production method as described in claim 1, which is characterized in that
O- methyl-isourea disulfate and oleum, concentrated nitric acid nitration reaction, obtain reaction solution；It specifically includes: in reaction kettle 115% oleum of middle addition cools down temperature control at -10-0 DEG C, the O- methyl-isourea disulfate being then added；Heat preservation- 10-0 DEG C, 98% sulfuric acid and nitric acid mixed acid is then added；Then, reaction solution is aged 24 hours at -5 DEG C.
8. O- methyl-N methyl-N '-nitro isourea production method as described in claim 1, which is characterized in that
Reaction solution is added in the cooling water of temperature control, crystallization, after need to carry out:
Filter centrifugation rejection filter obtains product O- methyl N-nitro isourea；
Concentrated hydrochloric acid and methylamine water solution methylation reaction are added in O- methyl N-nitro isourea；
Sub-cooled crystallization；
Filtering, filter cake are washed with ice water；
It is dried to obtain target product O- methyl-N-methyl-N '-nitro isourea.
9. a kind of utilize O- methyl-N methyl-N ' described in claim 1~8 any one-nitro isourea production method production O- methyl-N methyl-N '-nitro isourea.
CN201910527330.9A 2019-06-18 2019-06-18 A kind of O- methyl-N methyl-N '-nitro isourea production method Pending CN110317152A (en)

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Application publication date: 20191011