CN103626654B - One prepares the method for 2,4-D dimethylamine salt raw pesticide - Google Patents
One prepares the method for 2,4-D dimethylamine salt raw pesticide Download PDFInfo
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- CN103626654B CN103626654B CN201310696475.4A CN201310696475A CN103626654B CN 103626654 B CN103626654 B CN 103626654B CN 201310696475 A CN201310696475 A CN 201310696475A CN 103626654 B CN103626654 B CN 103626654B
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- 238000000034 method Methods 0.000 title claims abstract description 39
- IUQJDHJVPLLKFL-UHFFFAOYSA-N 2-(2,4-dichlorophenoxy)acetate;dimethylazanium Chemical compound CNC.OC(=O)COC1=CC=C(Cl)C=C1Cl IUQJDHJVPLLKFL-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 239000000575 pesticide Substances 0.000 title claims abstract description 16
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims abstract description 210
- 239000003814 drug Substances 0.000 claims abstract description 31
- 239000007788 liquid Substances 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 239000005631 2,4-Dichlorophenoxyacetic acid Substances 0.000 claims abstract description 20
- 125000002147 dimethylamino group Chemical class [H]C([H])([H])N(*)C([H])([H])[H] 0.000 claims abstract description 10
- 238000009413 insulation Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000012423 maintenance Methods 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 description 14
- 238000007664 blowing Methods 0.000 description 14
- 241000196324 Embryophyta Species 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000005945 translocation Effects 0.000 description 2
- 240000001592 Amaranthus caudatus Species 0.000 description 1
- 235000009328 Amaranthus caudatus Nutrition 0.000 description 1
- 240000006122 Chenopodium album Species 0.000 description 1
- 235000009344 Chenopodium album Nutrition 0.000 description 1
- 244000058871 Echinochloa crus-galli Species 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 108091005461 Nucleic proteins Proteins 0.000 description 1
- 235000007199 Panicum miliaceum Nutrition 0.000 description 1
- 244000292697 Polygonum aviculare Species 0.000 description 1
- 235000006386 Polygonum aviculare Nutrition 0.000 description 1
- 235000002594 Solanum nigrum Nutrition 0.000 description 1
- 240000002307 Solanum ptychanthum Species 0.000 description 1
- 241001251949 Xanthium sibiricum Species 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 235000012735 amaranth Nutrition 0.000 description 1
- 239000004178 amaranth Substances 0.000 description 1
- -1 amine salt Chemical class 0.000 description 1
- 244000022185 broomcorn panic Species 0.000 description 1
- 230000032823 cell division Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000003054 hormonal effect Effects 0.000 description 1
- 102000039446 nucleic acids Human genes 0.000 description 1
- 108020004707 nucleic acids Proteins 0.000 description 1
- 150000007523 nucleic acids Chemical class 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- QIIPQYDSKRYMFG-UHFFFAOYSA-N phenyl hydrogen carbonate Chemical compound OC(=O)OC1=CC=CC=C1 QIIPQYDSKRYMFG-UHFFFAOYSA-N 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 230000005080 plant death Effects 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses one and prepare 2, the method of 4-D dimethylamine salt raw pesticide, is characterized in that comprising the following steps: former for 2,4-D medicine is put into container, instill liquid dimethyl amine when constantly stirring or pass into gaseous state dimethylamine, continue insulation reaction after dimethylamine adds, after reaction, the unreacted dimethylamine of removing, obtains 2,4-D dimethylamine salt wet feed, wet feed is dried, obtains 2,4-D dimethylamine salt raw pesticide.Present invention process is simple, raw material is easy to get, and direct reaction obtain 2,4-D dimethylamine salt raw pesticide, and without the need to concentrating, the step such as crystallization, good product quality, yield is high, whole process three-waste free discharge, and production capacity is high, and the feature of environmental protection is good, and mass-producing using value is high.
Description
Technical field
The present invention relates to the method that one prepares 2,4-D dimethylamine salt raw pesticide, belong to preparation technique of pesticide field.
Background technology
2,4-D is phenoxy carboxylic acid selectivity Uptake and translocation hormonal weedicide, and sterling is white crystal, and in water, solubleness is very little, is soluble in the organic solvent such as ethanol, benzene, but its sodium salt, amine salt are then very easily water-soluble.There is stronger Uptake and translocation, growth and development of plants can be suppressed when lower concentration, cause and occur deformity until dead, be mainly used in cauline leaf process after seedling, Different Effects is produced to the synthesis of nucleic acid and protein, vegetative point is stopped growing, young leaflet tablet not tensible, normally carrying out of inhibited photosynthesis, be transmitted to the medicament of plant bottom, promote abnormal cell division, the tip of a root expands, lose receptivity, cause the distortion of stem stalk, deformity, screen casing blocks, and phloem destroys, organism transport is obstructed, and causes Plant death.2,4-D class weedicide has excellent preventive effect, as weeds such as three-coloured amaranth, knotweed, lamb's-quarters, black nightshade, Siberian cocklebur, barnyard grass, Herba Setariae Viridis, lady's-grass, broomcorn millets to 1 year of Soybean Field and other leguminous plants fields or perennial gramineous weeds and some broadleaf weeds.
At present, market is sold 2,4-D main formulations are the missible oil of its ester class and the aqua of dimethylamine salt.Because the organic solvent in missible oil is inflammable and environmental pollution can be caused comparatively large, the proportion of this formulation in pesticide preparation declines year by year in recent years.And 2, although 4-D dimethylamine aqua belongs to environmentally friendly formulation, very easily there is crystallization in the aqua of high density when low temperature, although lower concentration aqua there will not be crystallization, add packaging and transportation cost, also limit it to a certain extent and use.Our company successfully develops the environmentally friendly preparation about 2,4-D dimethylamine salt for 2012---2,4-D dimethylamine salt soluble granula, and declared patent, application number is 201210016942.X.
At present, for 2, less disclosed in the technology of preparing of 4-D dimethylamine salt, applicant has applied for that in 2009 " a kind of preparation method of 2,4-D dimethylamine salt bulk drug " by name, application number are the patent of invention of 200910020721.8, and this patent is with dimethylamine agueous solution and 2,4-D former medicine reaction preparation 2,4-D dimethylamine salt, needs to carry out the aftertreatment such as concentrating under reduced pressure, decrease temperature crystalline to reaction solution and just can obtain 2,4-D required dimethylamine salts after reaction.The method production process is more loaded down with trivial details, and operation steps is more, and production capacity is also lower, no matter all there is certain deficiency on production cost or on safety and environmental protection.
Summary of the invention
The object of this invention is to provide the method that one prepares 2,4-D dimethylamine salt raw pesticide, the method is simple, raw material is easy to get, be that the synthesis of 2,4-D dimethylamine salt provides a kind of new thinking, be more conducive to 2,4-D dimethylamine salt subsequent product, applying of such as soluble granula.
The present invention is achieved by the following measures:
One prepares 2, the method of 4-D dimethylamine salt raw pesticide, is characterized in that comprising the following steps: former for 2,4-D medicine is put into container, instill liquid dimethyl amine when constantly stirring or pass into gaseous state dimethylamine, continue insulation reaction after dimethylamine adds, after reaction, the unreacted dimethylamine of removing, obtains 2,4-D dimethylamine salt wet feed, wet feed is dried, obtains 2,4-D dimethylamine salt raw pesticide.
The present invention replaces dimethylamine agueous solution with dimethylamine raw material that is liquid or gaseous state, and make reaction more succinct, aftertreatment is more convenient, three-waste free discharge, meets environmental requirement, is cleanly production route.Use liquid dimethyl amine faster than gaseous state dimethylamine speed of response.
In aforesaid method, following step can also be increased: after adding the former medicine of 2,4-D, first add a small amount of water, then instill liquid dimethyl amine or pass into gaseous state dimethylamine.The add-on of water, not to be advisable higher than 10% of the former medicine quality of 2,4-D, is preferably 5%.
In aforesaid method, react for confined reaction.
In aforesaid method, the mol ratio of 2,4-D and dimethylamine is 1:1-1.5, preferred 1:1.02, when selecting 1:1.02, best on cost etc. considers.
In aforesaid method, the thermal creep stress 30-130 DEG C adding dimethylamine and add rear insulation reaction is advisable.The too low reaction being unfavorable for material of temperature, the too high meeting of temperature causes the decomposition of product, therefore preferred 50-85 DEG C.
In aforesaid method, adopt liquid dimethyl amine and gaseous state dimethylamine slightly difference in step.When adopting liquid dimethyl amine, instillation liquid dimethyl amine needs 10min-5h, drips insulation reaction 5min-60min after dimethylamine; Time for adding more fast response is stronger, reaction times longer material reaction more thorough.When adopting gaseous state dimethylamine, constantly pass into dimethylamine until led to, pass in process and keep system pressure to bear pressure lower than container, led to rear insulation reaction 5-60min.
The increase of reaction pressure is conducive to the raising of speed of response, but also to consider equipment bear pressure and safety control.At dropping liquid dimethylamine or pass in gaseous state dimethylamine process, generally keep system pressure to be 0-1MPa, be preferably 0.2-1MPa, the pressure in insulation reaction stage and dimethylamine complete time pressure difference little.When using liquid dimethyl amine, system pressure, by the rate of addition of dimethylamine, dripping quantity and controlling reaction temperature, can adjust this tittle as required and carry out under suitable speed to make reaction.
In aforesaid method, in liquid dimethyl amine, the content of dimethylamine is 70-100wt%, and other compositions are mainly water.Dimethylamine content 100% in gaseous state dimethylamine.
In aforesaid method, during oven dry, carry out under normal or reduced pressure, vacuum tightness is 0 ~-0.1Mpa, preferably-0.09MPa, and temperature is 30-110 DEG C, preferably 50 DEG C.
The present invention has the following advantages:
1, simple, the raw material of present invention process is easy to get.
The steps such as the method 2, recorded in patent 200910020721.8 needs to prepare, distill, saltout, filter, oven dry could finally obtain 2,4-D dimethylamine salt raw pesticide, production process is more loaded down with trivial details, and yield can only maintain about 80%, and the inventive method adopts 2, the former medicine of 4-D and dimethylamine directly react, and operation steps is simple, improves 2, the yield of 4-D dimethylamine salt, yield can reach more than 99%, and unnecessary dimethylamine can be recycled, and powerlessness is wasted.
3, whole preparation is simple, and can realize automatization, continuous prodution, three-waste free discharge, production capacity is high, and the feature of environmental protection is good, and mass-producing using value is high.
4, products obtained therefrom quality is good, yield 99%-99.8%, and during 2,4-D former medicine content 99.5% used, product purity is up to 99.5%, and during 2,4-D former medicine content 98% used, product purity also can reach 97.5%-98.0%, is applicable to scale production application.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, it is to be understood that following explanation is only to explain the present invention, do not limit its content.If no special instructions, following material content is mass content.
Following embodiment prepares 2, the method of 4-D dimethylamine salt raw pesticide is: by 2, airtight container put into by the former medicine of 4-D, do not add water or adds a small amount of water, instills liquid dimethyl amine or pass into gaseous state dimethylamine to make it fully react under the condition be uninterruptedly uniformly mixed, continue to stir after adding dimethylamine and carry out insulation reaction again, and then vacuumize dimethylamine unnecessary in eliminating material, obtain 2,4-D dimethylamine salt wet feed, then 2,4-D dimethylamine salt raw pesticide can be obtained through oven dry.Enumerate several preferred embodiment of the present invention below.Following pressure is gauge pressure.
embodiment 1
By 1000g 2, the former medicine of 4-D (content 98%) drops in kneader, drip sterling liquid dimethyl amine (content 100%) 203.5g under sealed conditions, time for adding is 2h, control when dripping dimethylamine that system pressure is 0.3MPa, temperature is 65 DEG C, 30min is incubated again after dropwising, opening emptying vacuumizes then blowing in unnecessary dimethylamine suction absorption tower, dry at the pressure of-0.08MPa and 50 DEG C, obtain that content is 98.2% 2,4-D dimethylamine salt 1194.0g, yield is 99.4%.
embodiment 2
By 1000g 2, the former medicine of 4-D (content 98%) drops in kneader, drip sterling liquid dimethyl amine (content 100%) 299.3g under sealed conditions, time for adding is 5h, control when dripping dimethylamine that system pressure is 1.0MPa, temperature is 130 DEG C, 60min is incubated again after dropwising, opening emptying vacuumizes then blowing in unnecessary dimethylamine suction absorption tower, dry at the pressure of-0.08MPa and 110 DEG C, obtain that content is 98.2% 2,4-D dimethylamine salt 1194.0g, yield is 99.4%.
embodiment 3
By 1000g 2, the former medicine of 4-D (content 99%) drops in kneader, then the 100g that adds water drips sterling liquid dimethyl amine (content 100%) 201.6g under sealed conditions, time for adding is 1h, control when dripping dimethylamine that system pressure is 0.7MPa, temperature is 85 DEG C, 50min is incubated again after dropwising, opening emptying vacuumizes then blowing in unnecessary dimethylamine suction absorption tower, dry at the pressure of-0.08MPa and 80 DEG C, obtain that content is 99.2% 2,4-D dimethylamine salt 1198.8g, yield is 99.8%.
embodiment 4
By 1000g 2, the former medicine of 4-D (content 99%) drops in kneader, then the 10g that adds water drips liquid dimethylamine (content 70%) 293g under sealed conditions, time for adding is 90min, control when dripping dimethylamine that system pressure is 0MPa, temperature is 75 DEG C, 5min is incubated again after dropwising, opening emptying vacuumizes then blowing in unnecessary dimethylamine suction absorption tower, dry at normal pressure and 60 DEG C, obtain that content is 99.3% 2,4-D dimethylamine salt 1197.2g, yield is 99.8%.
embodiment 5
By 1000g 2, the former medicine of 4-D (content 99%) drops in kneader, then the 50g that adds water drips liquid dimethylamine (content 70%) 283g under sealed conditions, time for adding is 50min, control when dripping dimethylamine that system pressure is 0.4MPa, temperature is 30 DEG C, 15min is incubated again after dropwising, opening emptying vacuumizes then blowing in unnecessary dimethylamine suction absorption tower, dry at-0.1MPa and 30 DEG C, obtain that content is 99.1% 2,4-D dimethylamine salt 1197.6g, yield is 99.6%.
embodiment 6
By 1000g 2, the former medicine of 4-D (content 99%) drops in kneader, then liquid dimethylamine (content 90%) 293g is dripped under sealed conditions, time for adding is 105min, control when dripping dimethylamine that system pressure is 0.3MPa, temperature is 30 DEG C, 40min is incubated again after dropwising, opening emptying vacuumizes then blowing in unnecessary dimethylamine suction absorption tower, dry at normal pressure and 50 DEG C, obtain that content is 99.2% 2,4-D dimethylamine salt 1197.1g, yield is 99.66%.
embodiment 7
By 1000g 2, the former medicine of 4-D (content 99%) drops in kneader, then sterling liquid dimethyl amine (content 100%) 209.6g is dripped under sealed conditions, time for adding is 2.5h, control when dripping dimethylamine that system pressure is 0.4MPa, temperature is 130 DEG C, 20min is incubated again after dropwising, opening emptying vacuumizes then blowing in unnecessary dimethylamine suction absorption tower, dry at normal pressure and 110 DEG C, obtain that content is 99.0% 2,4-D dimethylamine salt 1198.0g, yield is 99.5%.
embodiment 8
By 1000g 2, the former medicine of 4-D (content 99%) drops in kneader, then liquid dimethylamine (content 95%) 268.6g is dripped under sealed conditions, time for adding is 4h, control when dripping dimethylamine that system pressure is 0.1MPa, temperature is 55 DEG C, 30min is incubated again after dropwising, opening emptying vacuumizes then blowing in unnecessary dimethylamine suction absorption tower, dry at the pressure of-0.06MPa and 50 DEG C, obtain that content is 99.2% 2,4-D dimethylamine salt 1197.5g, yield is 99.69%.
embodiment 9
By 1000g 2, the former medicine of 4-D (content 99%) drops in kneader, then sterling liquid dimethyl amine (content 100%) 220.5g is dripped under sealed conditions, time for adding is 1h, control when dripping dimethylamine that system pressure is 0.3MPa, temperature is 85 DEG C, 50min is incubated again after dropwising, opening emptying vacuumizes then blowing in unnecessary dimethylamine suction absorption tower, dry at the pressure of-0.07MPa and 60 DEG C, obtain that content is 99.1% 2,4-D dimethylamine salt 1198.2g, yield is 99.65%.
embodiment 10
By 1000g 2, the former medicine of 4-D (content 98%) drops in kneader, then sterling liquid dimethyl amine (content 100%) 210g is dripped under sealed conditions, time for adding is 1h, control when dripping dimethylamine that system pressure is 0.7MPa, temperature is 80 DEG C, 30min is incubated again after dropwising, opening emptying vacuumizes then blowing in unnecessary dimethylamine suction absorption tower, dry at the pressure of-0.02MPa and 50 DEG C, obtain that content is 97.5% 2,4-D dimethylamine salt 1197.7g, yield is 99%.
embodiment 11
By 1000g 2, the former medicine of 4-D (content 98%) drops in kneader, then sterling liquid dimethyl amine (content 100%) 215g is dripped under sealed conditions, time for adding is 2h, control when dripping dimethylamine that system pressure is 0.4MPa, temperature is 60 DEG C, 30min is incubated again after dropwising, opening emptying vacuumizes then blowing in unnecessary dimethylamine suction absorption tower, dry at the pressure of-0.05MPa and 40 DEG C, obtain that content is 97.8% 2,4-D dimethylamine salt 1198.2g, yield is 99.35%.
embodiment 12
By 1000g 2, the former medicine of 4-D (content 99.5%) drops in kneader, add water 50g, then sterling gaseous state dimethylamine (content 100%) 206.7g is passed under sealed conditions, the logical dimethylamine time is 2h, when logical dimethylamine, control system pressure 0.6MPa, temperature are 70 DEG C, 30min is incubated again after having led to, opening emptying vacuumizes then blowing in unnecessary dimethylamine suction absorption tower, dry at the pressure of-0.05MPa and 75 DEG C, obtain 2, the 4-D dimethylamine salt 1192g that content is 99.5%, yield is 99.0%.
embodiment 13
By 1000g 2, the former medicine of 4-D (content 99.5%) drops in kneader, then sterling liquid dimethyl amine (content 100%) 230g is dripped under sealed conditions, time for adding is 2h, control when dripping dimethylamine that system pressure is 0.6MPa, temperature is 70 DEG C, 30min is incubated again after dropwising, opening emptying vacuumizes then blowing in unnecessary dimethylamine suction absorption tower, dry at the pressure of-0.05MPa and 70 DEG C, obtain that content is 99.5% 2,4-D dimethylamine salt 1198g, yield is 99.53%.
embodiment 14
By 1000g 2, the former medicine of 4-D (content 99.5%) drops in kneader, add water 100g, then sterling gaseous state dimethylamine (content 100%) 303.9g is passed under sealed conditions, the logical dimethylamine time is 2.5h, when logical dimethylamine, control system pressure 7.6MPa, temperature are 70 DEG C, be incubated 30min again, opening emptying vacuumizes then blowing in unnecessary dimethylamine suction absorption tower, dry at the pressure of-0.04MPa and 85 DEG C, obtain 2, the 4-D dimethylamine salt 1194g that content is 99.5%, yield is 99.2%.
Claims (11)
1. prepare 2 for one kind, the method of 4-D dimethylamine salt raw pesticide, is characterized in that comprising the following steps: former for 2,4-D medicine is put into kneader, instill liquid dimethyl amine when constantly stirring or pass into gaseous state dimethylamine, continue insulation reaction after dimethylamine adds, after reaction, the unreacted dimethylamine of removing, obtains 2,4-D dimethylamine salt wet feed, wet feed is dried, obtains 2,4-D dimethylamine salt raw pesticide; Reaction is confined reaction, and drip liquid dimethylamine or pass in gaseous state dimethylamine process, maintenance system pressure is 0-1MPa;
In liquid dimethyl amine, the content of dimethylamine is 70-100wt%.
2. method according to claim 1, is characterized in that: after adding the former medicine of 2,4-D, first add a small amount of water, then instills liquid dimethyl amine or pass into gaseous state dimethylamine, and the add-on of water is not higher than 10% of the former medicine quality of 2,4-D.
3. method according to claim 2, is characterized in that: the add-on of water is not higher than 5% of the former medicine quality of 2,4-D.
4. the method according to claim 1,2 or 3, is characterized in that: the mol ratio of 2,4-D and dimethylamine is 1:1-1.5.
5. method according to claim 4, is characterized in that: the mol ratio of 2,4-D and dimethylamine is 1:1.02.
6. the method according to claim 1,2 or 3, is characterized in that: the temperature of reaction of the former medicine of 2,4-D and dimethylamine is 30-130 DEG C.
7. method according to claim 6, is characterized in that: the temperature of reaction of the former medicine of 2,4-D and dimethylamine is 50-85 DEG C.
8. the method according to claim 1,2 or 3, is characterized in that: when adopting liquid dimethyl amine, and instillation liquid dimethyl amine needs 10min-5h, drips insulation reaction 5min-60min after dimethylamine; When adopting gaseous state dimethylamine, constantly pass into dimethylamine until led to, pass in process and keep system pressure to bear pressure lower than container, led to rear insulation reaction 5-60min.
9. the method according to claim 1,2 or 3, is characterized in that: drip liquid dimethylamine or pass in gaseous state dimethylamine process, maintenance system pressure is 0.2-1MPa.
10. the method according to claim 1,2 or 3, is characterized in that: during oven dry, and pressure is 0 ~-0.1Mpa, and temperature is 30-110 DEG C.
11. methods according to claim 10, is characterized in that: during oven dry, pressure is-0.09MPa, and temperature is 50 DEG C.
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| CN105175249B (en) * | 2015-08-20 | 2017-07-21 | 弘峰(北海)合浦农药有限公司 | A kind of method for preparing 2,4 D dimethylamine salt solids |
| CN105949237B (en) * | 2016-07-14 | 2019-01-04 | 山东润博生物科技有限公司 | A kind of preparation method of glyphosate dimethylamine salt raw medicine |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4001006A (en) * | 1971-09-10 | 1977-01-04 | Kalo Laboratories, Inc. | Dialkylammonium-2,4-dichlorophenoxyacetates as plant growth regulators and the method of making same |
| CN101525288A (en) * | 2009-04-21 | 2009-09-09 | 山东潍坊润丰化工有限公司 | Preparation method of 2, 4-D dimethylamine salt material drug |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4001006A (en) * | 1971-09-10 | 1977-01-04 | Kalo Laboratories, Inc. | Dialkylammonium-2,4-dichlorophenoxyacetates as plant growth regulators and the method of making same |
| CN101525288A (en) * | 2009-04-21 | 2009-09-09 | 山东潍坊润丰化工有限公司 | Preparation method of 2, 4-D dimethylamine salt material drug |
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