CN106279005A - A kind of method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material - Google Patents
A kind of method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material Download PDFInfo
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/62—Oxygen or sulfur atoms
- C07D213/63—One oxygen atom
- C07D213/64—One oxygen atom attached in position 2 or 6
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Abstract
A kind of produce waste material, from trichloro pyridyl sodium alcoholate, the method reclaiming trichloro pyridyl sodium alcoholate, belong to chemical field, carrying out first time Basic fluxing raction including trichloro pyridyl sodium alcoholate being produced waste material with the mixing of the first alkali liquor, obtaining alkaline hydrolysis coarse fodder；Described alkaline hydrolysis coarse fodder and the second alkali liquor being mixed and carry out second time Basic fluxing raction, described second time Basic fluxing raction is 0.1～0.6MPa at pressure, and temperature is carried out under conditions of being 100～160 DEG C.Employing the method can high yield, highly purified recovery trichloro pyridyl sodium alcoholate.The method is simple to operate, and equipment requirements is the highest, and production cost is low, can be with large-scale use.The waste water obtained after processing by the method can be directly discharged in biochemistry pool, eliminates the trouble of process further, saves the expense that waste water processes.
Description
Technical field
The present invention relates to chemical field, produce recovery trichlorine waste material in particular to one from trichloro pyridyl sodium alcoholate
The method of pyridine sodium alkoxide.
Background technology
3,5,6-trichloropyridine-2-sodium alkoxide, are called for short trichloro pyridyl sodium alcoholate, are a kind of important industrial chemicals, synthesize especially
The important intermediate of the Multiple Pesticides such as organophosphorus insecticide chlopyrifos, chlorpyrifos-methyl, herbicide Triclopyr.Trichloro pyridyl sodium alcoholate
The technological process of production is mainly trichloro-acetic chloride and generates butyl chloride with acrylonitrile addition, and butyl chloride carries out cyclization and obtains pyridine-4
(1H)-one (hereinafter referred to as pyridone), pyridone generates sodium alkoxide in the basic conditions.The mistake of pyridone is generated in butyl chloride cyclization
Cheng Zhonghui produces substantial amounts of waste material, wherein fails the pyridone of separating-purifying containing more by-product 4 chloro pyridine and part, and relatively
Many acrylonitrile polymers impurity.And in waste treatment process, it is necessary to remove acrylonitrile polymer impurity and by 4 chloro pyridine
Convert with pyridone and recycle, to improve the ultimate yield of sodium alkoxide.
In prior art, by chemically or physically method by 4 chloro pyridine separating-purifying from waste material, then will be able to purify
After 4 chloro pyridine be converted into trichloro pyridyl sodium alcoholate.But the process of separating-purifying 4 chloro pyridine becomes from the waste material that impurity is numerous
This height, the time is long, and it is the most time-consuming that the solid 4 chloro pyridine purified out carries out alkaline hydrolysis, and yield is undesirable.Prior art
In, also have and realize waste disposal by catalyst, although such method productivity is pretty good, but the consumption of catalyst is not
Few, while a large amount of wastes causing catalyst, also can result in catalyst residual, the pesticide having catalyst to remain once is thrown
Enter to use, it is possible to by plants enriched and finally human body is damaged.
Summary of the invention
It is an object of the invention to provide a kind of side producing from trichloro pyridyl sodium alcoholate and reclaiming trichloro pyridyl sodium alcoholate waste material
Method, it can be removed trichloro pyridyl sodium alcoholate quickly and easily and produces in waste material unwanted impurity and useful component converted also
Recycling, recovering effect is good, and yield is high, and the trichloro pyridyl sodium alcoholate purity obtained is high.
Embodiments of the invention are achieved in that
A kind of method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material, including:
Trichloro pyridyl sodium alcoholate is produced waste material and the mixing of the first alkali liquor carries out Basic fluxing raction for the first time, obtain alkaline hydrolysis coarse fodder；
Alkaline hydrolysis coarse fodder and the second alkali liquor being mixed and carry out second time Basic fluxing raction, Basic fluxing raction is 0.1 at pressure for the second time
～0.6MPa, temperature is carried out under conditions of being 100～160 DEG C.
The embodiment of the present invention provides the benefit that: one of the present invention produces waste material from trichloro pyridyl sodium alcoholate and returns
The method receiving trichloro pyridyl sodium alcoholate includes Basic fluxing raction and second time Basic fluxing raction for the first time, can by first time Basic fluxing raction
Trichloro pyridyl sodium alcoholate is produced the pyridone in waste material it is converted into trichloro pyridyl sodium alcoholate with effective, then by high at high temperature
Trichloro pyridyl sodium alcoholate then can be produced the 4 chloro pyridine in waste material and be converted into trichloropyridine alcohol by the second time Basic fluxing raction of pressure
Sodium.If trichloro pyridyl sodium alcoholate directly produces waste material alkaline hydrolysis at high temperature under high pressure, trichloro pyridyl sodium alcoholate produces the pyridine in waste material
Ketone can have precedence over alkali reaction, consumes substantial amounts of alkali, has not enough time to the 4 chloro pyridine volatilization loss at high temperature under high pressure of reaction, makes
Become yield on the low side.The mode using substep alkaline hydrolysis then can be effectively prevented from this situation, the recovery trichloropyridine of high yield
Sodium alkoxide.Meanwhile, the waste water obtained after processing by the method can be directly discharged in biochemistry pool, eliminates the fiber crops of process further
Tired, save the expense that waste water processes.
Detailed description of the invention
For making the purpose of the embodiment of the present invention, technical scheme and advantage clearer, below will be in the embodiment of the present invention
Technical scheme be clearly and completely described.In embodiment, unreceipted actual conditions person, builds according to normal condition or manufacturer
The condition of view is carried out.Agents useful for same or instrument unreceipted production firm person, being can be by the commercially available conventional product bought and obtain
Product.
Below the method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material of the embodiment of the present invention is entered
Row illustrates.
A kind of method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material, comprises the following steps:
Step S1, produces waste material by trichloro pyridyl sodium alcoholate and the mixing of the first alkali liquor carries out Basic fluxing raction for the first time, obtains alkali
Solve coarse fodder.
In present pre-ferred embodiments, the first alkali liquor is the aqueous slkali of 10～40wt%.Preferably, aqueous slkali is by hydrogen-oxygen
Any one changed in sodium and potassium hydroxide is mixed to prepare with water.Aqueous slkali in this concentration range, ensure that Basic fluxing raction
It is smoothed out, avoids reacting excessively fierce simultaneously and cause temperature too high and cause the loss of 4 chloro pyridine.
In present pre-ferred embodiments, Basic fluxing raction is carried out in a kettle. for the first time, for the first time the temperature of Basic fluxing raction
Degree is 20～70 DEG C.This temperature has met pyridone, and to be converted into the reaction of trichloro pyridyl sodium alcoholate temperature required.The too high appearance of temperature
The volatilization easily causing 4 chloro pyridine is run off, and brings danger to experimental implementation simultaneously.
In present pre-ferred embodiments, the pH of Basic fluxing raction maintains 10～14 for the first time.Specifically, maintain pH permissible
Use the mode directly adding alkali or aqueous slkali.Pyridone is converted into the reaction of trichloro pyridyl sodium alcoholate it is necessary to have enough concentration
Alkali just can carry out, meeting that alkali concn is on the low side causes to react and is even difficult to react slowly.
In present pre-ferred embodiments, trichloro pyridyl sodium alcoholate is produced waste material and the mixing of the first alkali liquor is by trichloropyridine
Sodium alkoxide produces waste material and is added drop-wise in the first alkali liquor and is uniformly mixed.Use the mode of dropping, reaction can be prevented further
The high temperature that excessive velocities is brought rises, it is preferable that trichloro pyridyl sodium alcoholate produces waste material and is added dropwise to complete in 6～9h, dropping
After maintain stirring 1～4h.Stirring is possible to prevent the too high local temperature caused of local concentration too high, and reaction is produced
Raw even heat disperses away, maintains stablizing of reaction to carry out.
In present pre-ferred embodiments, after first time Basic fluxing raction, by filter pressing isolated alkaline hydrolysis coarse fodder.Pressure
Filter can remove most acrylonitrile polymer impurity, makes follow-up second time Basic fluxing raction more efficient.
Step S2, mixes alkaline hydrolysis coarse fodder and the second alkali liquor and carries out second time Basic fluxing raction, and Basic fluxing raction is in pressure for the second time
Power is 0.1～0.6MPa, and temperature is carried out under conditions of being 100～160 DEG C.
In present pre-ferred embodiments, the second alkali liquor is the aqueous slkali of 10～40wt%.Preferably, aqueous slkali is by hydrogen-oxygen
Any one changed in sodium and potassium hydroxide is mixed to prepare with water.Aqueous slkali in this concentration range, ensure that Basic fluxing raction
It is smoothed out.
Further, in other preferred embodiment of the present invention, Basic fluxing raction is carried out in high pressure base analysis still for the second time, adopts
Mode with gradient increased temperature boosting.Specifically, Basic fluxing raction includes high pressure alkaline hydrolysis for the first time for the second time: by thick for mixed alkaline hydrolysis
Material and the second alkali liquor are 0.1～0.5MPa at pressure, and temperature is to react 2～6h at 100～150 DEG C to obtain an alkaline hydrolysis material.Enter
One step ground, the second time high pressure alkaline hydrolysis after Basic fluxing raction also includes first time high pressure alkaline hydrolysis for the second time: in first time high pressure base
On the basis of solution, continuing increasing temperature and pressure, be 0.2～0.6MPa by alkaline hydrolysis material at pressure, temperature is anti-at 120～160 DEG C
2～4h are answered to obtain secondary alkaline hydrolysis material；The separated purification of secondary alkaline hydrolysis material obtains trichloro pyridyl sodium alcoholate.The mode of gradient increased temperature boosting
Effectively can adjust reaction condition according to the concentration of 4 chloro pyridine.In initial reaction stage, when 4 chloro pyridine concentration is bigger, Ying Cai
With relatively low pressure and temperature, the volatilization of 4 chloro pyridine is avoided to run off；And phase after the reaction, 4 chloro pyridine concentration is less
Time, then should use of a relatively high pressure and temperature, ensure that 4 chloro pyridine can convert completely.
In present pre-ferred embodiments, after secondary Basic fluxing raction, obtain trichloro pyridyl sodium alcoholate by filter pressing.Filter pressing energy
Remove reacted impurity and moisture further, obtain the trichloro pyridyl sodium alcoholate that purity is higher.
Below in conjunction with embodiment, inventive feature and performance are described in further detail.
Embodiment 1
A kind of method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material of the present embodiment offer:
In alkaline hydrolysis still, put into 15.0kg water and 7.5kg concentration is the sodium hydroxide solution of 30wt%, be uniformly mixed
Obtain the first alkali liquor.Open circulating condensing water, control alkaline hydrolysis temperature in the kettle and be not higher than 50 DEG C.Take trichloro pyridyl sodium alcoholate and produce waste material
4.5kg the most at the uniform velocity drips in 6～7h and enters in alkaline hydrolysis still.After dropping, take out after continuing reaction 1～2h and press
Filter, obtains alkaline hydrolysis crude product.During reaction, every 20min detects a pH, supplements sodium hydroxide solution in time and controls the pH of reaction
Between 10～12.
In high pressure base analysis still, put into 20kg water and 4.0kg solid sodium hydroxide, be uniformly mixed and obtain the second alkali liquor.
Alkaline hydrolysis crude product is joined in high pressure base analysis still, be forced into 0.1MPa, be warming up to 110 DEG C of reaction 3h and obtain an alkaline hydrolysis material.Will
Alkaline hydrolysis material repressurization, to 0.2MPa, is warming up to 120 DEG C of reaction 2h and obtains secondary alkaline hydrolysis material, press after being taken out by secondary alkaline hydrolysis material
Filter obtains trichloro pyridyl sodium alcoholate.
Embodiment 2
A kind of method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material of the present embodiment offer:
In alkaline hydrolysis still, put into 16.0kg water and 4.0kg sodium hydrate solid, be uniformly mixed and obtain the first alkali liquor.Beat
Open cycle condensed water, controls alkaline hydrolysis temperature in the kettle and is not higher than 55 DEG C.Take trichloro pyridyl sodium alcoholate and produce waste material 4.5kg in 7～8h
In the most at the uniform velocity dropping enters alkaline hydrolysis still.After dropping, take out after continuing reaction 2～3h and carry out filter pressing, obtain alkaline hydrolysis crude product.
During reaction, every 20min detects a pH, supplements sodium hydroxide solution in time and controls the pH of reaction between 12～14.
In high pressure base analysis still, put into 20kg water and 2.0kg solid sodium hydroxide, be uniformly mixed and obtain the second alkali liquor.
Alkaline hydrolysis crude product is joined in high pressure base analysis still, be forced into 0.2MPa, be warming up to 120 DEG C of reaction 5h and obtain an alkaline hydrolysis material.Will
Alkaline hydrolysis material repressurization, to 0.3MPa, is warming up to 130 DEG C of reaction 3h and obtains secondary alkaline hydrolysis material, press after being taken out by secondary alkaline hydrolysis material
Filter obtains trichloro pyridyl sodium alcoholate.
Embodiment 3
A kind of method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material of the present embodiment offer:
In alkaline hydrolysis still, put into 6.0kg water and the sodium hydroxide solution of 18.0kg 40wt%, be uniformly mixed and obtain the
One alkali liquor.Open circulating condensing water, control alkaline hydrolysis temperature in the kettle and be not higher than 60 DEG C.Take trichloro pyridyl sodium alcoholate and produce waste material 4.5kg
In in 8～9h, the most at the uniform velocity dropping enters alkaline hydrolysis still.After dropping, take out after continuing reaction 3～4h and carry out filter pressing, obtain
Alkaline hydrolysis crude product.During reaction, every 20min detects a pH, supplement in time sodium hydroxide solution and control the pH of reaction 11～
Between 13.
In high pressure base analysis still, put into 20kg water and 6.0kg solid sodium hydroxide, be uniformly mixed and obtain the second alkali liquor.
Alkaline hydrolysis crude product is joined in high pressure base analysis still, be forced into 0.4MPa, be warming up to 140 DEG C of reaction 6h and obtain an alkaline hydrolysis material.Will
Alkaline hydrolysis material repressurization, to 0.5MPa, is warming up to 150 DEG C of reaction 4h and obtains secondary alkaline hydrolysis material, press after being taken out by secondary alkaline hydrolysis material
Filter obtains trichloro pyridyl sodium alcoholate.
Embodiment 4
A kind of method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material of the present embodiment offer:
In alkaline hydrolysis still, put into 12.0kg water and 8.0kg sodium hydrate solid, be uniformly mixed and obtain the first alkali liquor.Beat
Open cycle condensed water, controls alkaline hydrolysis temperature in the kettle and is not higher than 50 DEG C.Take trichloro pyridyl sodium alcoholate and produce waste material 4.5kg in 7～8h
In the most at the uniform velocity dropping enters alkaline hydrolysis still.After dropping, take out after continuing reaction 2～3h and carry out filter pressing, obtain alkaline hydrolysis crude product.
During reaction, every 20min detects a pH, supplements sodium hydroxide solution in time and controls the pH of reaction between 12～13.
In high pressure base analysis still, put into 20kg water and 8.0kg solid sodium hydroxide, be uniformly mixed and obtain the second alkali liquor.
Alkaline hydrolysis crude product is joined in high pressure base analysis still, be forced into 0.3MPa, be warming up to 130 DEG C of reaction 5h and obtain an alkaline hydrolysis material.Will
Alkaline hydrolysis material repressurization, to 0.4MPa, is warming up to 140 DEG C of reaction 3h and obtains secondary alkaline hydrolysis material, press after being taken out by secondary alkaline hydrolysis material
Filter obtains trichloro pyridyl sodium alcoholate.
Embodiment 5
A kind of method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material of the present embodiment offer:
In alkaline hydrolysis still, put into 20kg 20wt% potassium hydroxide solution, be uniformly mixed and obtain the first alkali liquor.Open and follow
Ring condensed water, controls alkaline hydrolysis temperature in the kettle and is not higher than 70 DEG C.Take trichloro pyridyl sodium alcoholate production waste material 4.5kg slow in 7～8h
In at the uniform velocity dropping enters alkaline hydrolysis still.After dropping, take out after continuing reaction 2～3h and carry out filter pressing, obtain alkaline hydrolysis crude product.Reaction
Period, every 20min detects a pH, supplements sodium hydroxide solution in time and controls the pH of reaction between 10～12.
In high pressure base analysis still, put into 20kg water and 9.3kg solid potassium hydroxide, be uniformly mixed and obtain the second alkali liquor.
Alkaline hydrolysis crude product is joined in high pressure base analysis still, be forced into 0.5MPa, be warming up to 100 DEG C of reaction 3h and obtain an alkaline hydrolysis material.Will
Alkaline hydrolysis material repressurization, to 0.6MPa, is warming up to 110 DEG C of reaction 3h and obtains secondary alkaline hydrolysis material, press after being taken out by secondary alkaline hydrolysis material
Filter obtains trichloro pyridyl sodium alcoholate.
Embodiment 6
A kind of method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material of the present embodiment offer:
In alkaline hydrolysis still, put into 35kg 10wt% potassium hydroxide solution, be uniformly mixed and obtain the first alkali liquor.Open and follow
Ring condensed water, controls alkaline hydrolysis temperature in the kettle and is not higher than 60 DEG C.Take trichloro pyridyl sodium alcoholate production waste material 4.5kg slow in 7～8h
In at the uniform velocity dropping enters alkaline hydrolysis still.After dropping, take out after continuing reaction 3～4h and carry out filter pressing, obtain alkaline hydrolysis crude product.Reaction
Period, every 20min detects a pH, supplements sodium hydroxide solution in time and controls the pH of reaction between 11～13.
In high pressure base analysis still, put into 20kg water and 13.5kg solid potassium hydroxide, be uniformly mixed and obtain the second alkali
Liquid.Alkaline hydrolysis crude product is joined in high pressure base analysis still, be forced into 0.2MPa, be warming up to 150 DEG C of reaction 4h and obtain an alkaline hydrolysis material.
By an alkaline hydrolysis material repressurization to 0.3MPa, it is warming up to 160 DEG C of reaction 2h and obtains secondary alkaline hydrolysis material, after being taken out by secondary alkaline hydrolysis material
Filter pressing obtains trichloro pyridyl sodium alcoholate.
Comparative example 1
A kind of method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material of this comparative example offer:
In alkaline hydrolysis still, put into 15.0kg water and 7.5kg concentration is the sodium hydroxide solution of 30wt%, be uniformly mixed
Obtain alkali liquor.Open circulating condensing water, control alkaline hydrolysis temperature in the kettle and be not higher than 50 DEG C.Take trichloro pyridyl sodium alcoholate and produce waste material
4.5kg the most at the uniform velocity drips in 6～7h and enters in alkaline hydrolysis still.After dropping, take out after continuing reaction 1～2h and press
Filter, obtains trichloro pyridyl sodium alcoholate.During reaction, every 20min detects a pH, supplements sodium hydroxide solution in time and controls reaction
PH between 10～12.
Comparative example 2
A kind of method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material of this comparative example offer:
In high pressure base analysis still, put into 20kg water and 15kg solid sodium hydroxide, be uniformly mixed and obtain alkali liquor.Take three
Chloropyridine sodium alkoxide produces waste material 4.5kg and joins in high pressure base analysis still, is forced into 0.1MPa, is warming up to 110 DEG C of reaction 3h and obtains
Alkaline hydrolysis material.By an alkaline hydrolysis material repressurization to 0.2MPa, it is warming up to 120 DEG C of reaction 2h and obtains secondary alkaline hydrolysis material, by secondary
After alkaline hydrolysis material takes out, filter pressing obtains trichloro pyridyl sodium alcoholate.
Test example
According to embodiment 1～6 and producing from trichloro pyridyl sodium alcoholate of being used of comparative example 1～2 waste material reclaims trichlorine pyrrole
The method of pyridine sodium alkoxide, calculates yield, and compares the purity of final products, and concrete measuring method is as follows:
1. take a small amount of trichloro pyridyl sodium alcoholate production waste material and be configured to standard solution, use internal standard method, calculated by nuclear-magnetism
Trichloro pyridyl sodium alcoholate produces quality A and quality B of 4 chloro pyridine of pyridone in waste liquid, weighs final products trichloropyridine alcohol
Quality C of sodium, by following formula calculated yield: α=C/MC/(A/MA+B/MB), wherein, α is yield, MA, MB, MCIt is respectively pyridine
The molecular weight of ketone, 4 chloro pyridine and trichloro pyridyl sodium alcoholate.Result of calculation is shown in Table 1；
2. take a small amount of final products trichloro pyridyl sodium alcoholate and be configured to standard solution, use internal standard method, calculated by nuclear-magnetism
Quality D of pure trichloro pyridyl sodium alcoholate in final products, is weighed quality E of final products trichloro pyridyl sodium alcoholate, is calculated by following formula
Purity: β=D/E, wherein, β is purity.Result of calculation is shown in Table 1.
Table 1 embodiment 1～6 and the method for treating waste liquid contrast of comparative example 1～2
| Yield/% | Purity/% | |
| Embodiment 1 | 88.7 | 93 |
| Embodiment 2 | 99.4 | 89 |
| Embodiment 3 | 98.6 | 87 |
| Embodiment 4 | 95.5 | 88 |
| Embodiment 5 | 96.4 | 91 |
| Embodiment 6 | 93.3 | 85 |
| Comparative example 1 | 53.5 | 73 |
| Comparative example 2 | 73.4 | 86 |
In sum, trichloropyridine is reclaimed in producing from trichloro pyridyl sodium alcoholate that the embodiment of the present invention 1～6 is used waste material
The method of sodium alkoxide, it is possible to the major part in trichloro pyridyl sodium alcoholate production waste material be may utilize component and carry out trans-utilization, yield reaches
To more than 88.7%, and reclaim the product purity obtained more than 85%.Comparatively speaking, the normal pressure alkali that comparative example 1 is used
The method for treatment of waste material treatment effeciency solved is low, can only achieve 53.5%, due to the difficulty that not exclusively also result in separation converted,
The purity causing final products is the highest, only reaches 73%.And the waste disposal side of the High Temperature High Pressure alkaline hydrolysis that comparative example 2 is used
Method, although obtained the preferable product of purity, but in processing procedure, 4 chloro pyridine runs off serious, causes ultimate yield the highest,
Can only achieve 73.4%.
Can be seen that one of the present invention produces recovery three waste material from trichloro pyridyl sodium alcoholate by comparing above
The method of chloropyridine sodium alkoxide uses the mode of substep alkaline hydrolysis, can high yield, highly purified recovery trichloro pyridyl sodium alcoholate.The method
Simple to operate, equipment requirements is the highest, and production cost is low, can be with large-scale use.The waste water obtained after processing by the method can
To be directly discharged in biochemistry pool, eliminate the trouble of process further, save the expense that waste water processes.
Embodiments described above is a part of embodiment of the present invention rather than whole embodiments.The reality of the present invention
The detailed description executing example is not intended to limit the scope of claimed invention, but is merely representative of the selected enforcement of the present invention
Example.Based on the embodiment in the present invention, those of ordinary skill in the art are obtained under not making creative work premise
Every other embodiment, broadly falls into the scope of protection of the invention.
Claims (10)
1. one kind produces, from trichloro pyridyl sodium alcoholate, the method reclaiming trichloro pyridyl sodium alcoholate waste material, it is characterised in that including:
Trichloro pyridyl sodium alcoholate is produced waste material and the mixing of the first alkali liquor carries out Basic fluxing raction for the first time, obtain alkaline hydrolysis coarse fodder；
Described alkaline hydrolysis coarse fodder and the second alkali liquor being mixed and carry out second time Basic fluxing raction, described second time Basic fluxing raction at pressure is
0.1～0.6MPa, temperature is carried out under conditions of being 100～160 DEG C.
The method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material the most according to claim 1, it is special
Levying and be, described first alkali liquor and described second alkali liquor are the aqueous slkali of 10～40wt%；Described aqueous slkali is by sodium hydroxide
It is mixed to prepare with water with any one in potassium hydroxide.
The method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material the most according to claim 1, it is special
Levying and be, the reaction temperature of described first time Basic fluxing raction is 20～60 DEG C.
The method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material the most according to claim 1, it is special
Levying and be, the pH of described first time Basic fluxing raction maintains 10～14.
The method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material the most according to claim 1, it is special
Levying and be, described trichloro pyridyl sodium alcoholate is produced waste material mixing with described first alkali liquor is to produce described trichloro pyridyl sodium alcoholate to give up
Material is added drop-wise in 6-9h in described first alkali liquor and stirs, and drips complete follow-up continuous stirring 1-4h.
The method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material the most according to claim 1, it is special
Levying and be, described second time Basic fluxing raction uses the mode of gradient increased temperature boosting to divide multiple stage to carry out.
The method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material the most according to claim 6, it is special
Levying and be, described second time Basic fluxing raction includes high pressure alkaline hydrolysis for the first time: by mixed described alkaline hydrolysis coarse fodder and described second
Alkali liquor is 0.1～0.5MPa at pressure, and temperature is to react 2～6h at 100～150 DEG C to obtain an alkaline hydrolysis material.
The method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material the most according to claim 7, it is special
Levying and be, described second time Basic fluxing raction also includes the second time high pressure alkaline hydrolysis after described first time high pressure alkaline hydrolysis: described
For the first time on the basis of high pressure alkaline hydrolysis, continue increasing temperature and pressure, be 0.2～0.6MPa by a described alkaline hydrolysis material at pressure, temperature
It is to react 2～4h at 120～160 DEG C to obtain secondary alkaline hydrolysis material；The described secondary separated purification of alkaline hydrolysis material obtains described trichlorine pyrrole
Pyridine sodium alkoxide.
The method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material the most according to claim 1, it is special
Levy and be, after described first time Basic fluxing raction, by alkaline hydrolysis coarse fodder described in filter pressing isolated.
The method reclaiming trichloro pyridyl sodium alcoholate from trichloro pyridyl sodium alcoholate production waste material the most according to claim 1, it is special
Levy and be, after described second time Basic fluxing raction, by trichloro pyridyl sodium alcoholate described in filter pressing isolated.
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| CN113787082A (en) * | 2021-09-13 | 2021-12-14 | 江苏九九久科技有限公司 | Harmless treatment method for waste catalyst generated in synthetic process of trichloropyridine sodium alcoholate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1978429A (en) * | 2005-12-03 | 2007-06-13 | 徐国庆 | Method for treating 4 chloro pyridine in solvent |
| CN101941940A (en) * | 2010-07-27 | 2011-01-12 | 山西康得利精细化工有限公司 | 3,5,6-trichloropyridin-2-ol sodium high-boiling solid waste conversion method |
| CN104163789A (en) * | 2014-07-23 | 2014-11-26 | 安徽国星生物化学有限公司 | 3,5,6-trichloropyridin-2-ol sodium synthesis method |
-
2016
- 2016-08-17 CN CN201610679540.6A patent/CN106279005B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1978429A (en) * | 2005-12-03 | 2007-06-13 | 徐国庆 | Method for treating 4 chloro pyridine in solvent |
| CN101941940A (en) * | 2010-07-27 | 2011-01-12 | 山西康得利精细化工有限公司 | 3,5,6-trichloropyridin-2-ol sodium high-boiling solid waste conversion method |
| CN104163789A (en) * | 2014-07-23 | 2014-11-26 | 安徽国星生物化学有限公司 | 3,5,6-trichloropyridin-2-ol sodium synthesis method |
Non-Patent Citations (1)
| Title |
|---|
| 陈芳: "3,5,6-三氯吡啶-2-醇钠的合成工艺研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113787082A (en) * | 2021-09-13 | 2021-12-14 | 江苏九九久科技有限公司 | Harmless treatment method for waste catalyst generated in synthetic process of trichloropyridine sodium alcoholate |
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