CN102659530A - Continuous preparation method of herbicide intermediate of 2, 4-dichlorophenol - Google Patents
Continuous preparation method of herbicide intermediate of 2, 4-dichlorophenol Download PDFInfo
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- CN102659530A CN102659530A CN2012101281747A CN201210128174A CN102659530A CN 102659530 A CN102659530 A CN 102659530A CN 2012101281747 A CN2012101281747 A CN 2012101281747A CN 201210128174 A CN201210128174 A CN 201210128174A CN 102659530 A CN102659530 A CN 102659530A
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Abstract
The invention provides a continuous preparation method of an herbicide intermediate of 2, 4-dichlorophenol. The method includes the steps of continuously and reversely feeding phenol and chlorine gas in a mass ratio of 1: (1.4-1.5), subjecting fed materials to continuous chlorination reaction through a multistage chlorination tower, enabling reacted liquid materials to flow into a 2, 4-dichlorophenol receiving tank, and recycling the gas with water through a tail gas absorption tower. The continuous preparation method replaces existing batch type mode to prepare the intermediate 2, 4-dichlorophenol of 2, 4-D acid, operation is simple, safety of preparation is controllable, discharge of three wastes is reduced, power consumption is reduced, and unit time output is increased. Simultaneously, the preparation can further improve yield of products, and recycle by-product acid with concentration of 30.5% during the reaction.
Description
Technical field
The invention belongs to weedicide 2,4-D acid intermediates preparation field specifically is a kind of continuous preparation method of herbicide intermediate 2,4 dichloro phenol.
Background technology
2,4 dichlorophenoxyacetic acid is a kind of representative synthetic plant growth hormones (auxin), abbreviates 2 as, 4-D acid.2,4-D acid shows high activity in common plant growth hormones quantitative method, but in the oat elongation test that adopts plant growth hormones standard quantitative method, its effect is but quite low.And be purple when handling, therefore can make colorimetric assay with chromotropic acid (chromotropic acid).Having found 2 from Annemarie Zimmermann (P.W.Z immermann, 1942) etc., since the effect of 4-D acid, has been that many synthetic auxins at center are applied to agricultural development has rapidly been arranged with this material.This material is utilized as weedicide on a large scale and is prevented fruit early fallout agent etc.2,4-D acid can quite promptly be shifted in plant materials, according to the result of 14C spike, confirms that this material is according to carboxyl carbon, and the order of mesomethylene carbon is carried out catabolicly rapidly then, but its benzene nucleus part is not taken apart easily.Be sprinkled into 2 in the soil, 4-D acid can be Gram-negative coccus and flavobacterium aquatile bacteriums such as (Flavobacteriumaquatile) is decomposed.
Preparation 2 at present, the method for 4-D acid are that 2,4 dichlorophenoxyacetic acid sodium reacts with hydrochloric acid and directly synthesizes title product under the high temperature more than 80 ℃.2,4 dichlorophenoxyacetic acid sodium then is to prepare through the midbody 2,4 dichloro phenol.And domestic 2,4 dichloro phenol is that phenol and chlorine react directly synthetic title product under 50～60 ℃ temperature, generally adopts tank reactor and batch process to produce at present.The stirred-tank reactor complex structure, power consumption, cold consumption are big, and mixing of materials is inhomogeneous, and product quality can not get ensureing.Make the selection and the yield of chemosynthesis reaction not high, output is not high yet.
Summary of the invention
The objective of the invention is to provide according to the deficiency of prior art a kind of continuous preparation method of herbicide intermediate 2,4 dichloro phenol, it can cut down the consumption of energy, and improves yield, improves yield in unit time, and is easy to operate and production safety is controlled.
The present invention realizes through following technical scheme: a kind of herbicide intermediate 2; The continuous preparation method of 4-NSC 2879, its step comprises: with mass ratio is 1: behind the continuous backward feed of the phenol of 1.4-1.5 and chlorine, under 40-80 ℃ temperature; After multistage chlorination tower generation continuous chlorination reaction; Reacted liquid material is flowed into the 2,4 dichloro phenol receiving tank get final product, gas reclaims through water through tail gas absorber.
Said multistage chlorination tower is the 3-6 level.
After earlier the phenol heating being got into tail gas absorber absorption of residual chlorine residue gas in the fill process, in chloromix tower, mix also from bottom to top getting into the chlorination tower again with chlorine.
Said chlorination tower is packing tower or tray column.
Said chlorination tower is lass lining, graphite or liner tetrafluoro material.
The present invention replaces existing batch process to prepare weedicide 2 with the method for continous way, the midbody 2,4 dichloro phenol of 4-D acid; Easy to operate and production safety is controlled, can reduce working strength of workers greatly, improve production on-site environment; Improve reaction safety; Reduce the discharging of the three wastes, cut down the consumption of energy, improve yield in unit time.Simultaneously, preparation method of the present invention can also improve the yield of product, can reclaim simultaneously by-product concentration in the reaction and be 30.5% acid.
Embodiment
Below further specify the present invention through specific embodiment:
Instance 1
With quality is after 1000 parts phenol is heated to 40 ℃, gets into tail gas absorber absorption of residual chlorine residue gas, is that 1500 parts chlorine mixes in chloromix tower and also from bottom to top gets into the chlorination tower with quality again.Under 40-60 ℃ temperature, after 3 grades of board-like chlorination tower generation continuous chlorination reactions, reacted liquid material is flowed into the 2,4 dichloro phenol receiving tank get final product yield 94.19%.Said board-like chlorination tower is the lass lining material.
Tail gas gets into tail gas absorber behind separator, the hydrogenchloride that water reclaims in the tail gas is that concentration is 30.5% acid, yield 97.19%., most of chlorine is not absorbed by water, behind pump, syphon trap, moisture eliminator, returns chloromix tower through water.
Embodiment 2
With quality is after 1000 parts phenol is heated to 40 ℃, gets into tail gas absorber absorption of residual chlorine residue gas, is that 1450 parts chlorine mixes in chloromix tower and also from bottom to top gets into the chlorination tower with quality again.Under 60-70 ℃ temperature, after 5 grades of filler chlorination tower generation continuous chlorination reactions, reacted liquid material is flowed into the 2,4 dichloro phenol receiving tank get final product yield 95.33%.Said filler chlorination tower is a graphite material.
Tail gas gets into tail gas absorber behind separator, the hydrogenchloride that water reclaims in the tail gas is that concentration is 30.5% acid, yield 80.19%., most of chlorine is not absorbed by water, behind pump, syphon trap, moisture eliminator, returns chloromix tower through water.
Embodiment 3
With quality is after 1000 parts phenol is heated to 40 ℃, gets into tail gas absorber absorption of residual chlorine residue gas, is that 1400 parts chlorine mixes in chloromix tower and also from bottom to top gets into the chlorination tower with quality again.Under 70-80 ℃ temperature, after 6 grades of board-like chlorination tower generation continuous chlorination reactions, reacted liquid material is flowed into the 2,4 dichloro phenol receiving tank get final product yield 96.03%.Said board-like chlorination tower is a liner tetrafluoro material.
Tail gas gets into tail gas absorber behind separator, the hydrogenchloride that water reclaims in the tail gas is that concentration is 30.5% acid, yield 88.23%., most of chlorine is not absorbed by water, behind pump, syphon trap, moisture eliminator, returns chloromix tower through water.
Easy to operate and production safety is controlled with method of the present invention, can reduce working strength of workers greatly, improve production on-site environment, improve reaction safety, reduce the discharging of the three wastes, cut down the consumption of energy, improve yield in unit time.Simultaneously, preparation method of the present invention can also improve the yield of product, can reclaim simultaneously by-product concentration in the reaction and be 30.5% acid, has very strong practicality.
Claims (5)
1. herbicide intermediate 2; The continuous preparation method of 4-NSC 2879, its step comprises: with mass ratio is 1: behind the continuous backward feed of the phenol of 1.4-1.5 and chlorine, under 40-80 ℃ temperature; After multistage chlorination tower generation continuous chlorination reaction; Reacted liquid material is flowed into the 2,4 dichloro phenol receiving tank get final product, gas reclaims through water through tail gas absorber.
2. according to the continuous preparation method of the said herbicide intermediate 2,4 dichloro phenol of claim 1, it is characterized in that: said multistage chlorination tower is the 3-6 level.
3. according to the said herbicide intermediate 2 of claim 1; The continuous preparation method of 4-NSC 2879; It is characterized in that: after earlier the phenol heating being got into tail gas absorber absorption of residual chlorine residue gas in the fill process, in chloromix tower, mix also from bottom to top getting into the chlorination tower again with chlorine.
4. according to the continuous preparation method of the said herbicide intermediate 2,4 dichloro phenol of claim 1, it is characterized in that: said chlorination tower is packing tower or tray column.
5. according to the continuous preparation method of the said herbicide intermediate 2,4 dichloro phenol of claim 1, it is characterized in that: said chlorination tower is lass lining, graphite or liner tetrafluoro material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101281747A CN102659530A (en) | 2012-04-27 | 2012-04-27 | Continuous preparation method of herbicide intermediate of 2, 4-dichlorophenol |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012101281747A CN102659530A (en) | 2012-04-27 | 2012-04-27 | Continuous preparation method of herbicide intermediate of 2, 4-dichlorophenol |
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| CN102659530A true CN102659530A (en) | 2012-09-12 |
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| CN2012101281747A Pending CN102659530A (en) | 2012-04-27 | 2012-04-27 | Continuous preparation method of herbicide intermediate of 2, 4-dichlorophenol |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435453A (en) * | 2013-08-26 | 2013-12-11 | 东南大学 | Method for preparing 2,4-dichlorophenol through directional catalyzing and chlorination of phenol |
| CN104529757A (en) * | 2015-01-04 | 2015-04-22 | 南京慧博生物科技有限公司 | Method for continuously producing herbicide 2,4-dichlorophenoxyacetic acid |
| CN106883103A (en) * | 2017-04-25 | 2017-06-23 | 江西天宇化工有限公司 | A kind of preparation method of 2,4 chlorophenesic acid |
| CN108863729A (en) * | 2017-05-11 | 2018-11-23 | 中国石油化工股份有限公司 | A method of 2,4 dichloro phenol is prepared using microreactor |
| CN109096057A (en) * | 2018-10-15 | 2018-12-28 | 连云港恒贸化工有限公司 | A kind of technical process of tower continuous chlorination production parachlorophenol |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2947790A (en) * | 1958-01-14 | 1960-08-02 | Reichhold Chemicals Inc | Process for production of chlorinated phenols with recovery of hydrochloric acid |
| GB1195716A (en) * | 1967-07-19 | 1970-06-24 | Chemolimpex | Chlorinated Aromatic Compounds |
-
2012
- 2012-04-27 CN CN2012101281747A patent/CN102659530A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2947790A (en) * | 1958-01-14 | 1960-08-02 | Reichhold Chemicals Inc | Process for production of chlorinated phenols with recovery of hydrochloric acid |
| GB1195716A (en) * | 1967-07-19 | 1970-06-24 | Chemolimpex | Chlorinated Aromatic Compounds |
Non-Patent Citations (1)
| Title |
|---|
| 无名: "（四）利用余氯制2，4二氯苯酚", 《环境保护科学》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435453A (en) * | 2013-08-26 | 2013-12-11 | 东南大学 | Method for preparing 2,4-dichlorophenol through directional catalyzing and chlorination of phenol |
| CN104529757A (en) * | 2015-01-04 | 2015-04-22 | 南京慧博生物科技有限公司 | Method for continuously producing herbicide 2,4-dichlorophenoxyacetic acid |
| CN106883103A (en) * | 2017-04-25 | 2017-06-23 | 江西天宇化工有限公司 | A kind of preparation method of 2,4 chlorophenesic acid |
| CN106883103B (en) * | 2017-04-25 | 2020-06-09 | 江西天宇化工有限公司 | Preparation method of 2, 4-dichlorophenol |
| CN108863729A (en) * | 2017-05-11 | 2018-11-23 | 中国石油化工股份有限公司 | A method of 2,4 dichloro phenol is prepared using microreactor |
| CN109096057A (en) * | 2018-10-15 | 2018-12-28 | 连云港恒贸化工有限公司 | A kind of technical process of tower continuous chlorination production parachlorophenol |
| CN109096057B (en) * | 2018-10-15 | 2020-10-23 | 连云港恒贸化工有限公司 | Process for producing p-chlorophenol by tower-type continuous chlorination method |
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Application publication date: 20120912 |