CN108530284A - The preparation method of o-methyl-benzene fluoroacetic acid - Google Patents
The preparation method of o-methyl-benzene fluoroacetic acid Download PDFInfo
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- CN108530284A CN108530284A CN201810304499.3A CN201810304499A CN108530284A CN 108530284 A CN108530284 A CN 108530284A CN 201810304499 A CN201810304499 A CN 201810304499A CN 108530284 A CN108530284 A CN 108530284A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
- C07C51/367—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by introduction of functional groups containing oxygen only in singly bound form
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/64—Preparation of O-metal compounds with O-metal group bound to a carbon atom belonging to a six-membered aromatic ring
- C07C37/66—Preparation of O-metal compounds with O-metal group bound to a carbon atom belonging to a six-membered aromatic ring by conversion of hydroxy groups to O-metal groups
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/02—Preparation of carboxylic acids or their salts, halides or anhydrides from salts of carboxylic acids
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- 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
Abstract
The present invention provides a kind of preparation method of o-methyl-benzene fluoroacetic acid.Described method includes following steps：(1) o-cresol and aqueous slkali are subjected to phenol neutralization reaction and obtain solution A；(2) sodium chloroacetate and solution A are subjected to condensation reaction and obtain B solution；(3) B solution is distilled until the mass percentage content of the o-cresol in liquid phase stream is less than 1%, liquid phase stream enters next step；(4) under the action of the solvent, liquid phase stream is acidified, crystallizes and be obtained by filtration coarse crystal and filtrate, sodium chloroacetate return to step (2) of the filtrate as cycle, the coarse crystal is the mixed crystal for including o-methyl-benzene fluoroacetic acid and sodium chloride.The present invention replaces hydrochloric acid acidizing reaction using monoxone, reduces saturated sodium-chloride discharge of wastewater, also reduces the consumption of raw material.
Description
【Technical field】
The present invention relates to a kind of preparation methods of o-methyl-benzene fluoroacetic acid.
【Background technology】
Since nineteen forty-two, since 2,4-D are found and apply, phenoxy carboxylic acid compound as important herbicide
The characteristics of experienced development in more than 70 years, and being accepted extensively by feat of its highly selective and efficient spectrum etc. by people,
The place that do not replace is accounted in the current market share.The herbicide of phenoxy carboxylic acid is to belong to a kind of weeding of steroids
Agent, it has absorbability, can rapidly be absorbed by the root of plant and leaf portion and pass to plant whole body, causes raw inside weeds
Long hormone concentration is excessively high, and then influences cell growth and the metabolism of plant, can almost influence each of plant growth
Physiology course causes growth mechanism disorderly, eventually leads to weeds death.Phenoxy carboxylic acid derivatives herbicide is in addition to having the function of weeding
Except, also have the effect of growth regulating, is important the intermediate of pesticide and medicine synthesis.
- 4 chlorophenoxyacetic acid of 2- methyl (referred to as 2 first, 4 chlorine) is used as a kind of phenoxy carboxylic acid derivatives herbicide, is removed since its is excellent
Careless characteristic has very big production scale and production application demand in China.The production line of existing 2 first, 4 chlorine mainly has two
Kind, one is first chlorinations to be condensed again, and another kind is first to be condensed chlorination again, and the condensation reaction of 2 first, 4 chlorine is primarily referred to as adjacent first
Base phenol and monoxone or sodium chloroacetate are finally condensed shape under the catalysis of the highly basic such as sodium hydroxide by the dissolving of different solvents
At the process of o-methyl-benzene fluoroacetic acid compound, o-methyl-benzene fluoroacetic acid is the important intermediate for producing 2 first, 4 chlorine.
Application No. is the patents of CN201310220565.6 to disclose a kind of 2- first -4-chlorophenoxyacetic acid preparation process, packet
Include following steps：A., monoxone is dissolved in the water to obtain sodium chloroacetate solution is spare, the blending ratio of the two is 1:1；B. will
O-cresol and sodium hydroxide are placed in condensation reaction kettle and allocate, it is ensured that the allotment ratio of the two be 5: 1, reaction temperature be 55 DEG C-
65 DEG C, the reaction time is 0.4h~0.6h, final to obtain o-cresol sodium water solution；C. above-mentioned b after reaction, a institutes are added dropwise
The chloroacetic acid solution of acquisition ensures that the allotment ratio of chloroacetic acid solution and o-cresol sodium water solution is 1.05: 1, and reaction temperature is
110 DEG C -130 DEG C, the reaction time is 3.5h~4.5h, final to obtain 2- methyl phenoxy acetic acid sodium；D. terminate in above-mentioned c reactions
Afterwards, liquor natrii hypochloritis is added, ensures that the allotment ratio of 2- methyl phenoxy acetic acids sodium and liquor natrii hypochloritis are 1: 6, reaction temperature
Degree is 25 DEG C~35 DEG C, final to obtain 2- first -4-chlorophenoxyacetic acid sodium；E. above-mentioned d after reaction, by 2- first -4- chlorobenzenes
Fratol is transferred to from condensation reaction kettle in acid out kettle, and hydrochloric acid is added at this time, it is ensured that 2- first -4-chlorophenoxyacetic acid sodium and salt
The ratio of acid is 1: 1, final to obtain 2- first -4-chlorophenoxyacetic acid.The patent is acidified to obtain 2- first -4- chlorobenzene oxygen second by hydrochloric acid
Acid, the process generate the waste water of a large amount of sodium chloride-containings, while consuming hydrochloric acid and alkali.
【Invention content】
O-methyl-benzene fluoroacetic acid preparation method provided by the invention is acidified the chloroethene of generation using chloroethene acid instead of HCl
Sour sodium cycle is used for condensation reaction, while reducing saturated sodium-chloride discharge of wastewater, also reduces the consumption of raw material, reduces
Production cost.
The present invention provides a kind of preparation method of o-methyl-benzene fluoroacetic acid, and this method follows the steps below：
(1) o-cresol and aqueous slkali are subjected to phenol neutralization reaction obtain include reaction product o-cresol sodium solution A；
(2) condensation reaction that sodium chloroacetate and solution A carry out intermittently or serially is obtained including reaction product o-methyl-benzene
The B solution of Fratol；
(3) B solution described in batch distillation or continuous still until the o-cresol in liquid phase stream mass percentage content
Less than 1%, dense phenol is mutually back to step (1) after the main gaseous stream condensation layering including o-cresol, and main includes adjacent methyl
The liquid phase stream of sodiumphenoxyacetate enters next step；
(4) solvent and monoxone are added in liquid phase stream, under the action of the solvent, the liquid phase stream is acidified, ties
Coarse crystal and filtrate is obtained by filtration in crystalline substance, and the coarse crystal is the mixed crystal for including o-methyl-benzene fluoroacetic acid and sodium chloride, described
Filtrate is the aqueous solution for including sodium chloroacetate, sodium chloroacetate return to step (2) of the filtrate as cycle, wherein described molten
Agent is one or more kinds of mixtures of dichloroethanes, chlorobenzene and dimethyl carbonate, the acidification, the temperature control crystallized
It is 5~15 DEG C.
In one preferred embodiment of preparation method of o-methyl-benzene fluoroacetic acid provided by the invention, after the step (4)
Further include step (5), under preset temperature under the coarse crystal that is dissolved in water obtain the crystal of o-methyl-benzene fluoroacetic acid and contain chlorine
Change the aqueous solution of sodium.
In one preferred embodiment of preparation method of o-methyl-benzene fluoroacetic acid provided by the invention, in the step (1), institute
It is the NaOH solution or KOH solution that mass concentration is 30~50%, mole of the o-cresol and the aqueous slkali to state aqueous slkali
Proportioning is 1：(1.0~1.1).
In one preferred embodiment of preparation method of o-methyl-benzene fluoroacetic acid provided by the invention, in the step (1), institute
It is adiabatic reaction to state phenol neutralization reaction, and reaction temperature is 30~80 DEG C, and the reaction time is 0.5~2 hour.
In one preferred embodiment of preparation method of o-methyl-benzene fluoroacetic acid provided by the invention, in the step (2), institute
The reaction temperature for stating condensation reaction is 80~150 DEG C, and the reaction time is 3~6h, and reaction system pH controls are 8~10.
In one preferred embodiment of preparation method of o-methyl-benzene fluoroacetic acid provided by the invention, in the step (2), institute
State the sodium chloroacetate and fresh sodium chloroacetate that sodium chloroacetate includes cycle, and the sodium chloroacetate and the o-cresol in solution A
The molar ratio of sodium is (1~1.1)：1.
In one preferred embodiment of preparation method of o-methyl-benzene fluoroacetic acid provided by the invention, in the step (3), steam
It is 100~150 DEG C to evaporate temperature.
In one preferred embodiment of preparation method of o-methyl-benzene fluoroacetic acid provided by the invention, in the step (4), institute
The pH value for stating the reaction system of acidification reaction is controlled 1~3.
In one preferred embodiment of preparation method of o-methyl-benzene fluoroacetic acid provided by the invention, the preset temperature is 0
DEG C~15 DEG C.
Compared to the relevant technologies, the preparation method of o-methyl-benzene fluoroacetic acid provided by the invention has the advantages that：
Acidification reaction of the present invention prepares hydrochloric acid of the raw material of o-methyl-benzene fluoroacetic acid using monoxone instead of the prior art, the chloroethene of generation
The step of sour sodium is recycled back into condensation reaction is used as condensation reaction raw material to participate in condensation reaction and prepares o-methyl-benzene fluoroacetic acid again
Sodium, on the one hand, 1 mole of o-methyl-benzene fluoroacetic acid of synthesis can reduce the generation of 1 mole nacl, reduce saturated sodium-chloride waste water
Discharge；On the other hand, the sodium chloroacetate that acidification reaction generates recycles, it is possible to reduce the raw material alkali soluble of synthesis of chloroacetic acid sodium
The dosage of liquid reduces cost of material.
【Description of the drawings】
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing, wherein：
Fig. 1 is the process flow diagram of the preparation method of o-methyl-benzene fluoroacetic acid provided by the invention.
【Specific implementation mode】
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that the described embodiments are merely a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts all other
Embodiment shall fall within the protection scope of the present invention.
Referring to Fig. 1, a kind of method preparing o-methyl-benzene fluoroacetic acid, the method are as follows：
Step 1: phenol neutralization reaction synthesizing o-cresol sodium
O-cresol and aqueous slkali are subjected to phenol neutralization reaction obtain include reaction product o-cresol sodium solution A；It is wherein adjacent
Cresols includes the raw material o-cresol newly provided and the o-cresol through subsequent step separation cycle, by the adjacent first that will have neither part nor lot in reaction
Phenol is recycled back to step 1, can reduce production cost, while can also reduce the processing cost of phenol wastewater.
Aqueous slkali is the NaOH solution or KOH solution that mass concentration is 30~50%, and the o-cresol and the alkali soluble
The mol ratio of liquid is 1：(1.0~1.1).
The phenol neutralization reaction is adiabatic reaction, and reaction temperature is 30~80 DEG C, and the reaction time is 0.5~2 hour.
Step 2: condensation reaction synthesizes o-methyl-benzene Fratol
The contracting of solution A and sodium chloroacetate progress intermittently or serially including reaction product o-cresol sodium that step 1 is generated
The B solution for including reaction product o-methyl-benzene Fratol is obtained by the reaction in conjunction；The wherein described sodium chloroacetate includes by subsequent step
The sodium chloroacetate of recycling and fresh sodium chloroacetate, and the sodium chloroacetate and the o-cresol sodium in solution A rub
You are than being (1~1.1)：1.
Specifically, fresh sodium chloroacetate solution is obtained by monoxone and aqueous slkali progress neutralization reaction, synthesis of chloroacetic acid
The reaction condition of sodium is:The mol ratio of the monoxone and the aqueous slkali is 1：(1.0~1.1), reaction temperature be 10~
20 DEG C, wherein aqueous slkali is the NaOH solution or KOH solution that mass concentration is 30~50%.
Preferably, the reaction temperature of the condensation reaction is 80~150 DEG C, and the reaction time is 3~6h, pH controls 8~
10。
Shown in the equation of condensation reaction following (1)：
Step 3: distillation B solution separation o-cresol and o-methyl-benzene Fratol
B solution described in batch distillation or continuous still is until the mass percentage content of the o-cresol in liquid phase stream is less than
1%, dense phenol is mutually back to step (1) after the main gaseous stream condensation layering including o-cresol, includes mainly o-methyl-benzene oxygen
The liquid phase stream of sodium acetate enters next step.
Preferably, B solution described in batch distillation or continuous still until the o-cresol in liquid phase stream mass percent
Content is less than 0.5%.
Preferably, vapo(u)rizing temperature is 100~150 DEG C.
Step 4: liquid phase stream is acidified, crystallizes, being obtained by filtration the mixed crystal of o-methyl-benzene fluoroacetic acid and sodium chloride
After o-cresol separation in B solution, liquid phase stream is cooled to room temperature, then solvent is added in liquid phase stream
And monoxone, under the action of the solvent, the liquid phase stream is acidified, crystallize, coarse crystal and filtrate, the coarse-grain is obtained by filtration
Body is the mixed crystal for including o-methyl-benzene fluoroacetic acid and sodium chloride, and the filtrate is the aqueous solution for including sodium chloroacetate, described
Filtrate utilizes again as the sodium chloroacetate return to step two of cycle, wherein the solvent is dichloroethanes, chlorobenzene and carbonic acid two
One or more kinds of mixtures of methyl esters, the acidification, the temperature control crystallized are 5~15 DEG C；
Preferably, the pH value of the reaction system of the acidification reaction is controlled using monoxone within the scope of 1~3.
Acidification reaction of the present invention prepares o-methyl-benzene fluoroacetic acid, and the hydrochloric acid of the prior art is replaced using monoxone, generation
Sodium chloroacetate is recycled back into the step of condensation reaction, is used as condensation reaction raw material to participate in condensation reaction again and prepares o-methyl-benzene oxygen
Sodium acetate, on the one hand, the generation that 1 mole of o-methyl-benzene fluoroacetic acid of synthesis can reduce by 1 mole nacl is (i.e. of the invention only to contract
1 mole nacl can be generated by closing reaction, and prior art condensation reaction and acidification reaction can generate 1 mole nacl), it reduces
The discharge of saturated sodium-chloride waste water；On the other hand, the sodium chloroacetate that acidification reaction generates can recycle, and reduce synthesis chloroethene
The dosage of the raw material aqueous slkali of sour sodium reduces cost of material.It is existing using hydrochloric acid as the acidification reaction equation of raw material such as (2) institute
Show, it is shown as the reaction equation of the acidification of raw material such as (3) using monoxone：
Step 5: the coarse crystal that is dissolved in water under preset temperature obtains o-methyl-benzene fluoroacetic acid crystal
0 DEG C~15 DEG C coarse crystals that are dissolved in water obtain o-methyl-benzene fluoroacetic acid crystal and sodium chloride-containing it is water-soluble
Liquid.The aqueous solution of sodium chloride-containing is used as discharge of wastewater after processing.
It should be noted that the preparation method of o-methyl-benzene fluoroacetic acid provided by the invention can be that batch process can also
For continuous process.
Embodiment 1
The sodium hydroxide that 108 grams of o-cresols and 135 gram mass scores are 30% is placed in phenol neutralization reactor and is carried out absolutely
Thermal response obtains solution A, and reaction temperature is raised to 70 DEG C from room temperature, 1 hour reaction time；Simultaneously by 113 grams of monoxones and 160 grams
Sodium chloroacetate solution is obtained by the reaction at 10 DEG C in the sodium hydroxide that mass fraction is 30%；Solution A is mixed with sodium chloroacetate solution
Reaction, control temperature is at 100 DEG C, and the pH value for adjusting reaction system is 8, and reaction obtains B solution in 5 hours, at this time o-cresol
Content is 3%, and B solution is distilled at 140 DEG C, until the mass percentage content of o-cresol is reduced to 0.6% in solution, then
Liquid phase stream is cooled to room temperature, dichloroethanes is added and makees solvent, and monoxone is added and is reacted at 15 DEG C, control is anti-
It is 3 to answer system pH, after reaction, the mixed crystal containing o-methyl-benzene fluoroacetic acid and sodium chloride is obtained by filtration in reaction solution,
Solvent is mutually recycled for next group acidification reaction, and the fresh sodium chloroacetate solution mixing circulation of filtrate and supplement is anti-to lower batch
Liquid is answered, abovementioned steps are repeated.
Embodiment 2
The sodium hydroxide that 108 grams of 2,4- chlorophenesic acids and 135 gram mass scores are 30% is placed in phenol neutralization reactor
It carries out adiabatic reaction and obtains solution A, reaction temperature is raised to 70 DEG C from room temperature, 1 hour reaction time；Simultaneously by 142 grams of monoxones
Sodium chloroacetate solution is obtained by the reaction at 20 DEG C in the sodium hydroxide for being 32% with 187.5 gram mass scores, by solution A and sodium chloroacetate
Solution hybrid reaction, control temperature is at 90 DEG C, and the pH value for adjusting reaction system is 9, and reaction obtains B solution in 6 hours, adjacent at this time
The content of cresols is 2.3%, and B solution is distilled at 110 DEG C, until the mass percentage content of o-cresol is reduced in solution
0.7%, then liquid phase stream is cooled to room temperature, dichloroethanes is added and makees solvent, and monoxone is added and is carried out at 15 DEG C instead
It answers, control reaction system pH is 1, and after reaction, reaction solution is obtained by filtration containing o-methyl-benzene fluoroacetic acid and sodium chloride
Mixed crystal, solvent is mutually recycled for next group acidification reaction, by the fresh sodium chloroacetate solution mixing circulation of filtrate and supplement
To lower batch reaction solution, abovementioned steps are repeated.
Embodiment 3
The sodium hydroxide that 108 grams of 2,4- chlorophenesic acids and 100 gram mass scores are 40% is placed in phenol neutralization reactor
It carries out adiabatic reaction and obtains solution A, reaction temperature is raised to 70 DEG C from room temperature, 1 hour reaction time；Simultaneously by 103 grams of monoxones
Sodium chloroacetate solution is obtained by the reaction at 15 DEG C in the sodium hydroxide for being 30% with 147 gram mass scores, and solution A is molten with sodium chloroacetate
Liquid hybrid reaction, control temperature is at 110 DEG C, and the pH value for adjusting reaction system is 10, and reaction obtains B solution in 5 hours, adjacent at this time
The content of cresols is 3.2%, and B solution is distilled at 150 DEG C until the mass percentage content of o-cresol is reduced in solution
0.5%, then liquid phase stream is cooled to room temperature, dimethyl carbonate is added and makees solvent, and monoxone is added and is carried out at 15 DEG C
Reaction, control reaction system pH is 1, and after reaction, reaction solution is obtained by filtration containing o-methyl-benzene fluoroacetic acid and sodium chloride
Mixed crystal, solvent mutually recycles for next group acidification reaction, filtrate mixed with the fresh sodium chloroacetate solution of supplement and is followed
Ring repeats abovementioned steps to lower batch reaction solution.
Embodiment 4
By the sodium hydroxide that 108 grams of 2,4- chlorophenesic acids and 88 gram mass scores are 50% be placed in phenol neutralization reactor into
Row adiabatic reaction obtains solution A, and reaction temperature is raised to 70 DEG C from room temperature, 1.5 hours reaction time；Simultaneously by 110 grams of monoxones
Sodium chloroacetate solution is obtained by the reaction at 15 DEG C in the sodium hydroxide for being 32% with 150 gram mass scores, and solution A is molten with sodium chloroacetate
Liquid hybrid reaction, control temperature is at 80 DEG C, and the pH value for adjusting reaction system is 10, and reaction obtains B solution in 5.5 hours, at this time
The content of o-cresol is 2.6%, and B solution is distilled at 110 DEG C until the mass percentage content of o-cresol is reduced in solution
0.3%, then liquid phase stream is cooled to room temperature, chlorobenzene is added and makees solvent, and monoxone is added and is reacted at 15 DEG C, controls
Reaction system pH processed is 1, after reaction, reaction solution is obtained by filtration to the mix-crystal containing o-methyl-benzene fluoroacetic acid and sodium chloride
Body, solvent is mutually recycled for next group acidification reaction, by the fresh sodium chloroacetate solution mixing circulation of filtrate and supplement to lower batch
Secondary response liquid repeats abovementioned steps.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of o-methyl-benzene fluoroacetic acid, which is characterized in that this method follows the steps below：
(1) o-cresol and aqueous slkali are subjected to phenol neutralization reaction obtain include reaction product o-cresol sodium solution A；
(2) condensation reaction that sodium chloroacetate and solution A carry out intermittently or serially is obtained including reaction product o-methyl-benzene oxygen second
The B solution of sour sodium；
(3) B solution described in batch distillation or continuous still is until the mass percentage content of the o-cresol in liquid phase stream is less than
1%, dense phenol is mutually back to step (1) after the main gaseous stream condensation layering including o-cresol, includes mainly o-methyl-benzene oxygen
The liquid phase stream of sodium acetate enters next step；
(4) solvent and monoxone are added in liquid phase stream, under the action of the solvent, the liquid phase stream is acidified, crystallizes, mistake
Filter obtains coarse crystal and filtrate, and the coarse crystal is the mixed crystal for including o-methyl-benzene fluoroacetic acid and sodium chloride, the filtrate
It is the aqueous solution for including sodium chloroacetate, sodium chloroacetate return to step (2) of the filtrate as cycle, wherein the solvent is
One or more kinds of mixtures of dichloroethanes, chlorobenzene and dimethyl carbonate, the acidification, the temperature control crystallized are 5
~15 DEG C.
2. the preparation method of o-methyl-benzene fluoroacetic acid according to claim 1, which is characterized in that after the step (4)
Further include step (5), the coarse crystal that is dissolved in water under preset temperature obtains the crystal and chloride containing of o-methyl-benzene fluoroacetic acid
The aqueous solution of sodium.
3. the preparation method of o-methyl-benzene fluoroacetic acid according to claim 1, which is characterized in that in the step (1), institute
It is the NaOH solution or KOH solution that mass concentration is 30~50%, mole of the o-cresol and the aqueous slkali to state aqueous slkali
Proportioning is 1：(1.0~1.1).
4. the preparation method of o-methyl-benzene fluoroacetic acid according to claim 3, which is characterized in that in the step (1), institute
It is adiabatic reaction to state phenol neutralization reaction, and reaction temperature is 30~80 DEG C, and the reaction time is 0.5~2 hour.
5. the preparation method of o-methyl-benzene fluoroacetic acid according to claim 1, which is characterized in that in the step (2), institute
The reaction temperature for stating condensation reaction is 80~150 DEG C, and the reaction time is 3~6h, and reaction system pH controls are 8~10.
6. the preparation method of o-methyl-benzene fluoroacetic acid according to claim 5, which is characterized in that in the step (2), institute
State the sodium chloroacetate and fresh sodium chloroacetate that sodium chloroacetate includes cycle, and the sodium chloroacetate and the o-cresol in solution A
The molar ratio of sodium is (1~1.1)：1.
7. the preparation method of o-methyl-benzene fluoroacetic acid according to claim 1, which is characterized in that in the step (3), steam
It is 100~150 DEG C to evaporate temperature.
8. the preparation method of o-methyl-benzene fluoroacetic acid according to claim 1, which is characterized in that in the step (4), institute
The pH value for stating the reaction system of acidification reaction is controlled 1~3.
9. the preparation method of o-methyl-benzene fluoroacetic acid according to claim 2, which is characterized in that in the step (5), institute
It is 0 DEG C~15 DEG C to state preset temperature.
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| CN113121335A (en) * | 2021-04-16 | 2021-07-16 | 宁夏格瑞精细化工有限公司 | Preparation method of 2, 4-dichlorophenoxyacetic acid |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1618785A (en) * | 2003-11-20 | 2005-05-25 | 张沈昌 | Production technology of 2-methyl-4-chloro-sodium phenoxy acetate |
| CN101967092A (en) * | 2010-07-02 | 2011-02-09 | 厦门市亨瑞生化有限公司 | Method for synthesizing 2,6-dimethyl phenoxyacetic acid |
| CN102285890A (en) * | 2011-05-19 | 2011-12-21 | 江苏健谷化工有限公司 | Preparation process of 2-methyl-4-dimethylamine chlorophenoxyacetate |
| CN103058855A (en) * | 2011-10-20 | 2013-04-24 | 上海泰禾化工有限公司 | Method for synthesizing phenoxyacetic acid derivative |
| CN103351295A (en) * | 2013-06-04 | 2013-10-16 | 安徽兴隆化工有限公司 | 2-methyl-4-chlorophenoxyacetic acid preparation technology |
| CN107266310A (en) * | 2017-07-20 | 2017-10-20 | 山东科源化工有限公司 | The preparation method of technique solid waste reduction technology is dripped in monoxone acidization synthesis 2,4 |
| CN107867992A (en) * | 2016-09-26 | 2018-04-03 | 青岛九洲千和机械有限公司 | A kind of method for synthesizing Phenoxiacetic acid derivatives |
-
2018
- 2018-04-08 CN CN201810304499.3A patent/CN108530284A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1618785A (en) * | 2003-11-20 | 2005-05-25 | 张沈昌 | Production technology of 2-methyl-4-chloro-sodium phenoxy acetate |
| CN101967092A (en) * | 2010-07-02 | 2011-02-09 | 厦门市亨瑞生化有限公司 | Method for synthesizing 2,6-dimethyl phenoxyacetic acid |
| CN102285890A (en) * | 2011-05-19 | 2011-12-21 | 江苏健谷化工有限公司 | Preparation process of 2-methyl-4-dimethylamine chlorophenoxyacetate |
| CN103058855A (en) * | 2011-10-20 | 2013-04-24 | 上海泰禾化工有限公司 | Method for synthesizing phenoxyacetic acid derivative |
| CN103351295A (en) * | 2013-06-04 | 2013-10-16 | 安徽兴隆化工有限公司 | 2-methyl-4-chlorophenoxyacetic acid preparation technology |
| CN107867992A (en) * | 2016-09-26 | 2018-04-03 | 青岛九洲千和机械有限公司 | A kind of method for synthesizing Phenoxiacetic acid derivatives |
| CN107266310A (en) * | 2017-07-20 | 2017-10-20 | 山东科源化工有限公司 | The preparation method of technique solid waste reduction technology is dripped in monoxone acidization synthesis 2,4 |
Cited By (1)
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| CN113121335A (en) * | 2021-04-16 | 2021-07-16 | 宁夏格瑞精细化工有限公司 | Preparation method of 2, 4-dichlorophenoxyacetic acid |
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