CN110041211A - A kind of recovery and treatment method of 4,4 '-diaminodiphenyl ether rectifying still bottom residues - Google Patents
A kind of recovery and treatment method of 4,4 '-diaminodiphenyl ether rectifying still bottom residues Download PDFInfo
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- CN110041211A CN110041211A CN201910344248.2A CN201910344248A CN110041211A CN 110041211 A CN110041211 A CN 110041211A CN 201910344248 A CN201910344248 A CN 201910344248A CN 110041211 A CN110041211 A CN 110041211A
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/10—Separation; Purification; Stabilisation; Use of additives
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Abstract
The present invention relates to the recovery technology fields of fine chemistry industry organic material, the specially recovery and treatment method of one kind 4,4'- diaminodiphenyl ether rectifying still bottom residue, comprising the following steps: (1) is crushed residue；(2) above-mentioned fragment is put into dissolution kettle, and solvent (3) is added into dissolution kettle and mix activated carbon of sorbent into dissolution kettle；(4) liquid in dissolution kettle is pumped into plate filter and is filtered；(5) cooling down is carried out in the crystallization kettle of negative nitrogen environment, then carries out centrifugal treating；(6) mother liquor for obtaining centrifugation distills；(7) vacuum drier is dried in vacuo；(8) crude product in step (7) is put into distillation kettle and carries out distillation processing.4,4'- diaminodiphenyl ether in the residue of rectifying still bottom extraction and application, and rate of recovery height again can not only have been saved resource, also achieve resource reclaim recycling, and effectively reduce the processing cost of dangerous waste by the present invention.
Description
Technical field
The invention belongs to the recovery technology fields of fine chemistry industry organic material, and in particular to one kind 4,4'- diamino hexichol
The recovery and treatment method of ether rectifying still bottom residue.
Background technique
4,4'- diaminodiphenyl ethers are as crosslinking agents such as raw material, additive, intermediates, for production specific function and property
The products such as plastics, resin, dyestuff, the fragrance of matter, and the new product of research and development more powerful and specific function and property, all occupy spy
Critical role that is different and can not be substituted is especially applied to the coating of wire and cable, the inside and outside insulation of heat proof cable, motor
High-end national defence equipment and the products for civilian use such as groove pads, and the layer insulation and capacitor of transformer, tape, circuit are printed, more
Special and important meaning.
The main production process of 4,4'- diaminodiphenyl ether at present are as follows: add 4,4'- dinitro diphenyl ether and solvent investment
In hydrogen reaction kettle, under 60 DEG C or more, palladium-carbon catalyst effect, hydrogenation reaction generates 4,4'- diaminodiphenyl ether, by knot
The processes such as brilliant, filtering, obtain thick 4,4'- diaminodiphenyl ether, since 4,4'- diaminodiphenyl ether is made using dimethyl acetamide
For solvent, rectifying column is had to pass through using rear dimethyl acetamide and recycles secondary use, when distillation is to 145 DEG C, rectifying tower reactor
Bottom can generate 5% or so black residue, these residues are handled as dangerous waste in the prior art, but due to residue ingredient
In containing 40% or so 4,4'- diaminodiphenyl ether, directly as dangerous waste processing when result in waste of resources, thus generate every year
Economic loss it is huge.
Therefore, it is necessary to be carried out for 4, the 4'- diaminodiphenyl ether in the residue of 4,4'- diaminodiphenyl ether rectifying still bottom
Recycling causes the wasting of resources and economic loss to solve the residue behind rectifying still bottom in the prior art directly as dangerous waste processing
The problem of.
Summary of the invention
The purpose of the present invention is to provide the recovery and treatment method of one kind 4,4'- diaminodiphenyl ether rectifying still bottom residue,
By the extraction and application, and rate of recovery height again of 4, the 4'- diaminodiphenyl ether in the residue of rectifying still bottom, resource has not only been saved,
Resource reclaim recycling is also achieved, and effectively reduces the processing cost of dangerous waste.
In order to achieve the above object, the present invention is achieved through the following technical solutions:
The recovery and treatment method of one kind 4,4'- diaminodiphenyl ether rectifying still bottom residue, comprising the following steps:
(1) residue that dimethylacetamide solvent recycling rectifying tower reactor bottom generates is broken into the fragment that granularity is less than 5cm；
(2) above-mentioned fragment is put into dissolution kettle, and solvent is added into dissolution kettle, after stirring 20-30min, Xiang Rong
It solves kettle collet and leads to steam, be heated to 60-70 DEG C, continue to stir 50-60min, fragment dissolves, 4,4'- diaminodiphenyl ethers
All dissolutions；
(3) activated carbon of sorbent is mixed into dissolution kettle, after mixing evenly standing sedimentation, and remove insoluble unadsorbed
Compare heavy seeds greatly；
(4) liquid in dissolution kettle is pumped into plate filter and is filtered, filter cake enters crystallization as dangerous waste processing, filtrate
In kettle；
(5) cooling down is carried out in the crystallization kettle of negative nitrogen environment, then opens the bottom valve of crystallization kettle, it will be in crystallization kettle
Material is put into centrifuge and carries out centrifugal treating；
(6) the obtained mother liquor of centrifugation is put to distilling in distillation still, recycling design is recycled；
(7) filter cake obtained after distillation is put into vacuum drier and is dried in vacuo, it is molten to remove crystallization therein
Agent obtains 4,4 '-diaminodiphenyl ether crude products；
(8) crude product in step (7) is put into distillation kettle, and controls distillation kettle temperature degree at 210-220 DEG C, vacuum degree
Control is in≤- 0.09Mpa, and the 10-15h that distils is to get after the recovery 4,4 '-diaminodiphenyl ethers.
It is more preferred, what the solvent in the step (2) was made of methanol and toluene 1:1 in mass ratio.
More preferred, the mass ratio of fragment and solvent in the step (2) is 1:2.5-3.5.
More preferred, the mass ratio of fragment and solvent in the step (2) is 1:3.
More preferred, the filter sizes of the plate filter in the step (4) are 0.8-1.2 μm.
It is more preferred, the distillation condition in the step (6) are as follows: vapo(u)rizing temperature is 75-80 DEG C, distillation time 2-3h.
It is more preferred, vacuum drying condition in the step (7) are as follows: temperature control at 94-98 DEG C, vacuum degree≤-
0.08Mp, dry 1.5-2.5h.
It is more preferred, vacuum drying condition in the step (7) are as follows: temperature control at 96 DEG C, vacuum degree≤-
0.08Mp, dry 2.0h.
Compared with prior art, the beneficial effects of the present invention are: the present invention can be by 4, the 4'- diamino in the residue of rectifying still bottom
Yl diphenyl ether extraction and application, and rate of recovery height again, has not only saved resource, also achieves resource reclaim recycling, and
The processing cost of dangerous waste is effectively reduced, additionally there is following remarkable advantage:
(1) present invention can effectively realize the separation of organic impurities in fragment by selection methanol and toluene as solvent, and
Impurity in dissolution kettle is adsorbed by the way that adsorbent is added, and sedimentation removing is carried out for not adsorbable fixed impurity, then
Adsorbent is filtered out by plate filter and adsorbate carries out filtration removing, then crystallisation by cooling centrifugal treating, removal 4,4'-
Liquid solvent and soluble impurity except diaminodiphenyl ether improve the rate of recovery；
(2) present invention is dried by using vacuum drier, can effectively remove 4,4'- diaminodiphenyl ether crude product
Recrystallisation solvent, and by way of vacuum sublimation, the impurity of 4,4'- diaminodiphenyl ether is removed, raising recycling is further increased
4,4'- diaminodiphenyl ether purity.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
The recovery and treatment method of 4, the 4'- diaminodiphenyl ether rectifying still bottom residue of the present embodiment, comprising the following steps:
(1) residue that dimethylacetamide solvent recycling rectifying tower reactor bottom generates is broken into the fragment that granularity is less than 5cm；
(2) it takes above-mentioned 300kg fragment to put into dissolution kettle, and 375kg methanol and 375kg first is added into dissolution kettle
Benzene after stirring 20min, leads to steam to dissolution kettle collet, is heated to 60 DEG C, continues to stir 50min, and fragment dissolves, and 4,4'-
Diaminodiphenyl ether all dissolves；
(3) activated carbon of sorbent is mixed into dissolution kettle, after mixing evenly standing sedimentation, and remove insoluble unadsorbed
Compare heavy seeds greatly；
(4) liquid in dissolution kettle is pumped into the plate filter that filter sizes are 0.8-1.2 μm and is filtered, filter cake conduct
Dangerous waste processing, filtrate enter in crystallization kettle；
(5) cooling down is carried out in the crystallization kettle of negative nitrogen environment, then opens the bottom valve of crystallization kettle, it will be in crystallization kettle
Material is put into centrifuge and carries out centrifugal treating；
(6) the obtained mother liquor of centrifugation is put to distilling in distillation still, vapo(u)rizing temperature control is at 75 DEG C, and distillation time 2h is molten
Agent recycling；
(7) filter cake obtained after distillation is put into vacuum drier and is dried in vacuo, temperature is controlled at 94 DEG C, very
Reciprocal of duty cycle≤- 0.08Mp, dry 1.5h, removes recrystallisation solvent therein, obtains 4,4'- diaminodiphenyl ether crude product；
(8) crude product in step (7) is put into distillation kettle, and controls distillation kettle temperature degree at 210 DEG C, vacuum degree control
In≤- 0.09Mpa, the 10-15h that distils is to get after the recovery 4,4 '-diaminodiphenyl ethers.
Embodiment 2
The recovery and treatment method of 4, the 4'- diaminodiphenyl ether rectifying still bottom residue of the present embodiment, comprising the following steps:
(1) residue that dimethylacetamide solvent recycling rectifying tower reactor bottom generates is broken into the fragment that granularity is less than 5cm；
(2) it takes above-mentioned 300kg fragment to put into dissolution kettle, and 525kg methanol and 525kg first is added into dissolution kettle
Benzene after stirring 30min, leads to steam to dissolution kettle collet, is heated to 70 DEG C, continues to stir 60min, and fragment dissolves, and 4,4'-
Diaminodiphenyl ether all dissolves；
(3) activated carbon of sorbent is mixed into dissolution kettle, after mixing evenly standing sedimentation, and remove insoluble unadsorbed
Compare heavy seeds greatly；
(4) liquid in dissolution kettle is pumped into the plate filter that filter sizes are 0.8-1.2 μm and is filtered, filter cake conduct
Dangerous waste processing, filtrate enter in crystallization kettle；
(5) cooling down is carried out in the crystallization kettle of negative nitrogen environment, then opens the bottom valve of crystallization kettle, it will be in crystallization kettle
Material is put into centrifuge and carries out centrifugal treating；
(6) the obtained mother liquor of centrifugation is put to distilling in distillation still, vapo(u)rizing temperature control is at 80 DEG C, and distillation time 3h is molten
Agent recycling；
(7) filter cake obtained after distillation is put into vacuum drier and is dried in vacuo, temperature is controlled at 98 DEG C, very
Reciprocal of duty cycle≤- 0.08Mp, dry 2.5h, removes recrystallisation solvent therein, obtains 4,4'- diaminodiphenyl ether crude product；
(8) crude product in step (7) is put into distillation kettle, and controls distillation kettle temperature degree at 220 DEG C, vacuum degree control
In≤- 0.09Mpa, the 15h that distils is to get after the recovery 4,4 '-diaminodiphenyl ethers.
Embodiment 3
The recovery and treatment method of 4, the 4'- diaminodiphenyl ether rectifying still bottom residue of the present embodiment, comprising the following steps:
(1) residue that dimethylacetamide solvent recycling rectifying tower reactor bottom generates is broken into the fragment that granularity is less than 5cm；
(2) it takes above-mentioned 300kg fragment to put into dissolution kettle, and 450kg methanol and 450kg first is added into dissolution kettle
Benzene after stirring 25min, leads to steam to dissolution kettle collet, is heated to 65 DEG C, continues to stir 55min, and fragment dissolves, and 4,4'-
Diaminodiphenyl ether all dissolves；
(3) activated carbon of sorbent is mixed into dissolution kettle, after mixing evenly standing sedimentation, and remove insoluble unadsorbed
Compare heavy seeds greatly；
(4) liquid in dissolution kettle is pumped into the plate filter that filter sizes are 0.8-1.2 μm and is filtered, filter cake conduct
Dangerous waste processing, filtrate enter in crystallization kettle；
(5) cooling down is carried out in the crystallization kettle of negative nitrogen environment, then opens the bottom valve of crystallization kettle, it will be in crystallization kettle
Material is put into centrifuge and carries out centrifugal treating；
(6) the obtained mother liquor of centrifugation to be put to distilling in distillation still, vapo(u)rizing temperature is controlled at 78 DEG C, distillation time 2.5h,
Solvent recovery cycle uses；
(7) filter cake obtained after distillation is put into vacuum drier and is dried in vacuo, temperature is controlled at 96 DEG C, very
Reciprocal of duty cycle≤- 0.08Mp, dry 2.0h, removes recrystallisation solvent therein, obtains 4,4'- diaminodiphenyl ether crude product；
(8) crude product in step (7) is put into distillation kettle, and controls distillation kettle temperature degree at 215 DEG C, vacuum degree control
In≤- 0.09Mpa, the 13h that distils is to get after the recovery 4,4 '-diaminodiphenyl ethers.
Embodiment 4
The recovery and treatment method of 4, the 4'- diaminodiphenyl ether rectifying still bottom residue of the present embodiment, comprising the following steps:
(1) residue that dimethylacetamide solvent recycling rectifying tower reactor bottom generates is broken into the fragment that granularity is less than 5cm；
(2) above-mentioned 300kg fragment is put into dissolution kettle, and 420kg methanol and 420kg first is added into dissolution kettle
Benzene after stirring 23min, leads to steam to dissolution kettle collet, is heated to 63 DEG C, continues to stir 52min, and fragment dissolves, and 4,4'-
Diaminodiphenyl ether all dissolves；
(3) activated carbon of sorbent is mixed into dissolution kettle, after mixing evenly standing sedimentation, and remove insoluble unadsorbed
Compare heavy seeds greatly；
(4) liquid in dissolution kettle is pumped into the plate filter that filter sizes are 0.8-1.2 μm and is filtered, filter cake conduct
Dangerous waste processing, filtrate enter in crystallization kettle；
(5) cooling down is carried out in the crystallization kettle of negative nitrogen environment, then opens the bottom valve of crystallization kettle, it will be in crystallization kettle
Material is put into centrifuge and carries out centrifugal treating；
(6) the obtained mother liquor of centrifugation to be put to distilling in distillation still, vapo(u)rizing temperature is controlled at 76 DEG C, distillation time 2.3h,
Solvent recovery cycle uses；
(7) filter cake obtained after distillation is put into vacuum drier and is dried in vacuo, temperature is controlled at 95 DEG C, very
Reciprocal of duty cycle≤- 0.08Mp, dry 1.8h, removes recrystallisation solvent therein, obtains 4,4'- diaminodiphenyl ether crude product；
(8) crude product in step (7) is put into distillation kettle, and controls distillation kettle temperature degree at 213 DEG C, vacuum degree control
In≤- 0.09Mpa, the 11h that distils is to get after the recovery 4,4 '-diaminodiphenyl ethers.
Embodiment 5
The recovery and treatment method of 4, the 4'- diaminodiphenyl ether rectifying still bottom residue of the present embodiment, comprising the following steps:
(1) residue that dimethylacetamide solvent recycling rectifying tower reactor bottom generates is broken into the fragment that granularity is less than 5cm；
(2) above-mentioned 300kg fragment is put into dissolution kettle, and 525kg methanol and 525kg first is added into dissolution kettle
Benzene after stirring 28min, leads to steam to dissolution kettle collet, is heated to 68 DEG C, continues to stir 57min, and fragment dissolves, and 4,4'-
Diaminodiphenyl ether all dissolves；
(3) activated carbon of sorbent is mixed into dissolution kettle, after mixing evenly standing sedimentation, and remove insoluble unadsorbed
Compare heavy seeds greatly；
(4) liquid in dissolution kettle is pumped into the plate filter that filter sizes are 0.8-1.2 μm and is filtered, filter cake conduct
Dangerous waste processing, filtrate enter in crystallization kettle；
(5) cooling down is carried out in the crystallization kettle of negative nitrogen environment, then opens the bottom valve of crystallization kettle, it will be in crystallization kettle
Material is put into centrifuge and carries out centrifugal treating；
(6) the obtained mother liquor of centrifugation to be put to distilling in distillation still, vapo(u)rizing temperature is controlled at 78 DEG C, distillation time 2.7h,
Solvent recovery cycle uses；
(7) filter cake obtained after distillation is put into vacuum drier and is dried in vacuo, temperature is controlled at 97 DEG C, very
Reciprocal of duty cycle≤- 0.08Mp, dry 2.2h, removes recrystallisation solvent therein, obtains 4,4'- diaminodiphenyl ether crude product；
(8) crude product in step (7) is put into distillation kettle, and controls distillation kettle temperature degree at 218 DEG C, vacuum degree control
In≤- 0.09Mpa, the 14h that distils is to get after the recovery 4,4 '-diaminodiphenyl ethers.
Experimental example
To 4,4 '-diaminodiphenyl ethers weighing (the 4,4 '-diamino in fragment in embodiment 1-5 recycled in embodiment 1-5
Hexichol ether content is 120kg), and its purity is detected with gas chromatography, specific test result is as shown in table 1:
Table 1
| Sample | Purity (%) | Weight (kg) | The rate of recovery (%) |
| Embodiment 1 | 99.83 | 112 | 93.33 |
| Embodiment 2 | 99.88 | 115 | 95.83 |
| Embodiment 3 | 99.92 | 117 | 97.50 |
| Embodiment 4 | 99.90 | 111 | 92.50 |
| Embodiment 5 | 99.81 | 114 | 95.00 |
As can be seen from Table 1, using the recovery processing of one kind 4,4'- diaminodiphenyl ether rectifying still bottom residue of the invention
Method can effectively recycle 4, the 4'- diaminodiphenyl ether in the residue of rectifying still bottom, and the rate of recovery is high, up to
97.50%, and 4, the 4'- diaminodiphenyl ether purity recycled is up to 99.92%.
In summary, the present invention provides the recovery and treatment method of one kind 4,4'- diaminodiphenyl ether rectifying still bottom residue, will
4,4'- diaminodiphenyl ether extraction and application, and rate of recovery height again in the residue of rectifying still bottom, has not only saved resource, also
Resource reclaim recycling is realized, and effectively reduces the processing cost of dangerous waste.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to aforementioned reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features.It is all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. one kind 4, the recovery and treatment method of 4'- diaminodiphenyl ether rectifying still bottom residue, which is characterized in that including following step
It is rapid:
(1) residue that dimethylacetamide solvent recycling rectifying tower reactor bottom generates is broken into the fragment that granularity is less than 5cm；
(2) above-mentioned fragment is put into dissolution kettle, and solvent is added into dissolution kettle, after stirring 20-30min, to dissolution kettle
Collet leads to steam, is heated to 60-70 DEG C, continues to stir 50-60min, and fragment dissolves, and 4,4'- diaminodiphenyl ethers are whole
Dissolution；
(3) activated carbon of sorbent is mixed into dissolution kettle, after mixing evenly standing sedimentation, and remove insoluble unadsorbed big
Compare heavy seeds；
(4) liquid in dissolution kettle is pumped into plate filter and is filtered, filter cake enters crystallization kettle as dangerous waste processing, filtrate
It is interior；
(5) cooling down is carried out in the crystallization kettle of negative nitrogen environment, the bottom valve of crystallization kettle is then opened, by the material in crystallization kettle
It is put into centrifuge and carries out centrifugal treating；
(6) the obtained mother liquor of centrifugation is put to distilling in distillation still, recycling design is recycled；
(7) filter cake obtained after distillation is put into vacuum drier and is dried in vacuo, removed recrystallisation solvent therein, obtain
To 4,4'- diaminodiphenyl ether crude product；
(8) crude product in step (7) is put into distillation kettle, and controls distillation kettle temperature degree at 210-220 DEG C, vacuum degree control
In≤- 0.09Mpa, the 10-15h that distils is to get after the recovery 4,4 '-diaminodiphenyl ethers.
2. the recovery and treatment method of 4,4'- diaminodiphenyl ether rectifying still bottom according to claim 1 residue, feature exist
In what the solvent in the step (2) was made of methanol and toluene 1:1 in mass ratio.
3. the recovery and treatment method of 4,4'- diaminodiphenyl ether rectifying still bottom according to claim 1 residue, feature exist
In the mass ratio of fragment and solvent in the step (2) is 1:2.5-3.5.
4. the recovery and treatment method of 4,4'- diaminodiphenyl ether rectifying still bottom according to claim 4 residue, feature exist
In the mass ratio of fragment and solvent in the step (2) is 1:3.
5. the recovery and treatment method of 4,4'- diaminodiphenyl ether rectifying still bottom according to claim 1 residue, feature exist
In the filter sizes of the plate filter in the step (4) are 0.8-1.2 μm.
6. the recovery and treatment method of 4,4'- diaminodiphenyl ether rectifying still bottom according to claim 1 residue, feature exist
In distillation condition in the step (6) are as follows: vapo(u)rizing temperature is 75-80 DEG C, distillation time 2-3h.
7. the recovery and treatment method of 4,4'- diaminodiphenyl ether rectifying still bottom according to claim 1 residue, feature exist
In vacuum drying condition in the step (7) are as follows: temperature control dries 1.5- in 94-98 DEG C, vacuum degree≤- 0.08Mp
2.5h。
8. the recovery and treatment method of 4,4'- diaminodiphenyl ether rectifying still bottom according to claim 7 residue, feature exist
In vacuum drying condition in the step (7) are as follows: temperature control dries 2.0h in 96 DEG C, vacuum degree≤- 0.08Mp.
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Cited By (1)
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