CN110015965A - A method of 4,4 '-diaminodiphenyl ether secondary crystallizations of production - Google Patents
A method of 4,4 '-diaminodiphenyl ether secondary crystallizations of production Download PDFInfo
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- CN110015965A CN110015965A CN201910344817.3A CN201910344817A CN110015965A CN 110015965 A CN110015965 A CN 110015965A CN 201910344817 A CN201910344817 A CN 201910344817A CN 110015965 A CN110015965 A CN 110015965A
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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
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Abstract
The present invention relates to the purification technique field of fine chemistry industry organic material, specially a kind of method for producing 4,4'- diaminodiphenyl ether secondary crystallization, comprising the following steps: (1) by mixed solvent and block 4,4'- diaminodiphenyl ether is put into dissolution kettle；(2) lead to steam to dissolution kettle collet；(3) liquid in dissolution kettle is pumped into filter press and is filtered；(4) activated carbon of sorbent is mixed into reaction kettle；(5) liquid in step (4) was pumped into millipore filter and was filtered；(6) circulating water cooling is passed through in crystallization kettle collet；(7) centrifuge centrifugal treating；(8) it is dried in vacuum drier.The impurity of bulk 4,4'- diaminodiphenyl ether can be completely separated out by the present invention, and 4, the 4'- diaminodiphenyl ether purity after purifying can be made up to 99.9% or more.
Description
Technical field
The invention belongs to the purification technique fields of fine chemistry industry organic material, and in particular to a kind of 4,4 '-diamino of production
The method of diphenyl ether secondary crystallization.
Background technique
4,4 '-diaminodiphenyl ethers (being commonly called as diamines) are a kind of fine chemical product of high added value, abbreviation ODA, molecule
Amount 200.24, white or Light yellow crystals, it is tasteless, 189-191 DEG C of fusing point, 218 DEG C of flash-point.4,4 '-diaminodiphenyl ethers are main
It is used to prepare heat-resistant plastic such as polyimide resin, polymaleimide resins, polyamide-imide resin, polyesterimide
Resin, epoxy resin, polyurethane etc., also serve as crosslinking agent.Curing agent as epoxy resin, solidfied material heat distortion temperature is high,
Thermostabilization is good, and chemical resistance and water resistance are excellent.It is also heat-resisting plastic polyamideimide resin, polyimides tree
The raw material of rouge, polymaleimide resins etc..
Traditional 4, the preparation method of 4 '-diaminodiphenyl ethers usually using methanol as solvent, and are dissolved at 125 DEG C
4,4 '-diaminodiphenyl ethers, after completely dissolution, then the crystallization that cools down obtains 4,4 '-diaminodiphenyl ether of crystalloid, but this method
The separated from impurities in 4,4 '-diaminodiphenyl ethers is not come out, therefore, obtained 4,4 '-diaminodiphenyl ethers it is pure
Degree is not very high, also, traditional handicraft is completed in a reaction kettle, and heating, cooling is for a long time in set of system
Operation, it is also larger to the damage of equipment.
In consideration of it, it is necessary to provide a kind of methods for producing 4,4 '-diaminodiphenyl ether secondary crystallizations, to solve existing skill
The problem of art.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for producing 4,4 '-diaminodiphenyl ether secondary crystallizations, can will be blocky
The impurity of 4,4 '-diaminodiphenyl ethers is completely separated out, and 4,4 '-diaminodiphenyl ether purity after purifying can be made up to 99.9%
More than.
In order to achieve the above object, the present invention is achieved through the following technical solutions:
A kind of method producing 4,4 '-diaminodiphenyl ether secondary crystallizations, comprising the following steps:
(1) mixed solvent is put into dissolution kettle, puts into 4,4 '-diamino hexichol of block into reaction kettle while stirring
Ether, 4, the 4 '-diaminodiphenyl ether of block of investment and the weight ratio of mixed solvent are 1:4.2-4.5, the valve that feeds intake are closed, to envelope
The dissolution kettle closed carries out repeatedly evacuating note nitrogen, to form airfree negative pressure nitrogen environment；
(2) lead to steam to dissolution kettle collet, be heated to 55-65 DEG C, continue to stir 40-50min, block 4,4 '-two
Amino-diphenylethers all dissolves；
(3) liquid in the dissolution kettle of step (2) is pumped into filter press and is filtered, and filtrate is transferred in reaction kettle；
(4) activated carbon of sorbent is mixed into reaction kettle, after mixing evenly, is staticly settled；
(5) liquid in step (4) was pumped into millipore filter and was filtered, the impurity for filtering out adsorbent and absorption turns
It send to crystallization kettle, and nitrogen filled protection is carried out to crystallization kettle；
(6) it is passed through circulating water cooling in crystallization kettle collet, when temperature is down to 25-35 DEG C, opens the bottom valve of crystallization kettle,
Material in crystallization kettle is put into suction filtration tank and is drained, brilliant solid 4,4 '-diaminodiphenyl ether is obtained；
(7) solid 4, the 4 '-diaminodiphenyl ether of crystalline substance in step (6) is put into a centrifuge, and added into centrifuge
Enter water, after stirring 10-20min, then carries out centrifugal treating；
(8) it in the filter cake investment vacuum drier for obtaining step (7) centrifugation, is dried to get 4,4 '-diaminos
Yl diphenyl ether.
Preferably, the mixed solvent in the step (1) is pressed the ratio of 1:1.2-1.6 by methanol and dimethyl acetamide
What example was formulated.
Preferably, the multiple evacuation note nitrogen in the step (1) is to vacuumize six times, add nitrogen five times, and guarantee
The heating of dissolution kettle collet is no more than 25 DEG C when vacuumizing.
Preferably, leading to steam in the step (2) to dissolution kettle collet, being heated to 60 DEG C, continue to stir
45min, 4,4 '-diaminodiphenyl ether of block all dissolve.
Preferably, the filter sizes of the millipore filter in the step (5) are 0.3-0.8 μm.
Preferably, the recirculated water flow velocity in the step (6) is 1.2-1.6L/min.
Preferably, vacuum drying condition in the step (8) are as follows: vacuum degree≤- 0.09Mpa, drying temperature 84-
88 DEG C, drying time 40-60min.
Preferably, vacuum drying condition in the step (8) are as follows: vacuum degree -0.08Mpa, 86 DEG C of drying temperature,
Drying time 50min.
Compared with prior art, the beneficial effects of the present invention are:
The impurity of blocky 4,4 '-diaminodiphenyl ethers can be completely separated out by the present invention, 4,4 '-two after can making purification
Amino-diphenylethers purity is up to 99.9% or more；
Present invention dissolution and crystallization process are carried out under closing, nitrogen environment, guarantee that 4,4 '-diaminodiphenyl ethers mention
The generation of other reactions and being mixed into for impurity are not had in pure procedure, thus 4,4 '-diaminodiphenyl ethers provide one preferably
Purification environment；
The present invention is filtered by filter press and millipore filter twice, can be by the impurity of blocky 4,4 '-diaminodiphenyl ethers
It is completely separated out, the purity after ensure that the purification of 4,4 '-diaminodiphenyl ethers.
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 method of 4, the 4 '-diaminodiphenyl ether secondary crystallization of production of the present embodiment, comprising the following steps:
(1) 1260kg mixed solvent is put into dissolution kettle, puts into 300kg block 4 into reaction kettle while stirring,
4 '-diaminodiphenyl ethers close the valve that feeds intake, and carry out repeatedly evacuating note nitrogen to closed dissolution kettle, to form airfree bear
Press nitrogen environment；
(2) lead to steam to dissolution kettle collet, be heated to 55 DEG C, continue to stir 40min, 4,4 '-diamino two of block
Phenylate all dissolves；
(3) liquid in the dissolution kettle of step (2) is pumped into filter press and is filtered, and filtrate is transferred in reaction kettle；
(4) activated carbon of sorbent is mixed into reaction kettle, after mixing evenly, is staticly settled；
(5) liquid in step (4) was pumped into millipore filter and was filtered, the impurity for filtering out adsorbent and absorption turns
It send to crystallization kettle, and nitrogen filled protection is carried out to crystallization kettle；
(6) it is passed through circulating water cooling in crystallization kettle collet, when temperature is down to 25 DEG C, opens the bottom valve of crystallization kettle, it will
Material in crystallization kettle, which is put into suction filtration tank, to be drained, and brilliant solid 4,4 '-diaminodiphenyl ether is obtained；
(7) solid 4, the 4 '-diaminodiphenyl ether of crystalline substance in step (6) is put into a centrifuge, and added into centrifuge
Enter water, after stirring 10min, then carries out centrifugal treating；
(8) it in the filter cake investment vacuum drier for obtaining step (7) centrifugation, is dried to get 4,4 '-diaminos
Yl diphenyl ether.
Wherein, the mixed solvent in the step (1) is formulated by methanol and dimethyl acetamide in the ratio of 1:1.2
's.
Wherein, the multiple evacuation note nitrogen in the step (1) is to vacuumize six times, is added nitrogen five times, and guarantee to vacuumize
When dissolution kettle collet heating be no more than 25 DEG C.
Wherein, the filter sizes of the millipore filter in the step (5) are 0.3-0.8 μm.
Wherein, the recirculated water flow velocity in the step (6) is 1.2L/min.
Wherein, vacuum drying condition in the step (8) are as follows: vacuum degree -0.06Mpa, 84 DEG C of drying temperature, when dry
Between 40min.
Obtained above 4,4 '-diaminodiphenyl ethers are detected into its purity, purity 99.92% with gas chromatography.
Embodiment 2
The method of 4, the 4 '-diaminodiphenyl ether secondary crystallization of production of the present embodiment, comprising the following steps:
(1) 1350kg mixed solvent is put into dissolution kettle, puts into 300kg block 4 into reaction kettle while stirring,
4 '-diaminodiphenyl ethers close the valve that feeds intake, and carry out repeatedly evacuating note nitrogen to closed dissolution kettle, to form airfree bear
Press nitrogen environment；
(2) lead to steam to dissolution kettle collet, be heated to 65 DEG C, continue to stir 50min, 4,4 '-diamino two of block
Phenylate all dissolves；
(3) liquid in the dissolution kettle of step (2) is pumped into filter press and is filtered, and filtrate is transferred in reaction kettle；
(4) activated carbon of sorbent is mixed into reaction kettle, after mixing evenly, is staticly settled；
(5) liquid in step (4) was pumped into millipore filter and was filtered, the impurity for filtering out adsorbent and absorption turns
It send to crystallization kettle, and nitrogen filled protection is carried out to crystallization kettle；
(6) it is passed through circulating water cooling in crystallization kettle collet, when temperature is down to 35 DEG C, opens the bottom valve of crystallization kettle, it will
Material in crystallization kettle, which is put into suction filtration tank, to be drained, and brilliant solid 4,4 '-diaminodiphenyl ether is obtained；
(7) solid 4, the 4 '-diaminodiphenyl ether of crystalline substance in step (6) is put into a centrifuge, and added into centrifuge
Enter water, after stirring 20min, then carries out centrifugal treating；
(8) it in the filter cake investment vacuum drier for obtaining step (7) centrifugation, is dried to get 4,4 '-diaminos
Yl diphenyl ether.
Wherein, the mixed solvent in the step (1) is formulated by methanol and dimethyl acetamide in the ratio of 1:1.6
's.
Wherein, the multiple evacuation note nitrogen in the step (1) is to vacuumize six times, is added nitrogen five times, and guarantee to vacuumize
When dissolution kettle collet heating be no more than 25 DEG C.
Wherein, the filter sizes of the millipore filter in the step (5) are 0.3-0.8 μm.
Wherein, the recirculated water flow velocity in the step (6) is 1.6L/min.
Wherein, vacuum drying condition in the step (8) are as follows: vacuum degree -0.09Mpa, 88 DEG C of drying temperature, when dry
Between 60min.
Obtained above 4,4 '-diaminodiphenyl ethers are detected into its purity, purity 99.94% with gas chromatography.
Embodiment 3
The method of 4, the 4 '-diaminodiphenyl ether secondary crystallization of production of the present embodiment, comprising the following steps:
(1) 1300kg mixed solvent is put into dissolution kettle, puts into 300kg block 4 into reaction kettle while stirring,
4 '-diaminodiphenyl ethers close the valve that feeds intake, and carry out repeatedly evacuating note nitrogen to closed dissolution kettle, to form airfree bear
Press nitrogen environment；
(2) lead to steam to dissolution kettle collet, be heated to 60 DEG C, continue to stir 45min, 4,4 '-diamino two of block
Phenylate all dissolves；
(3) liquid in the dissolution kettle of step (2) is pumped into filter press and is filtered, and filtrate is transferred in reaction kettle；
(4) activated carbon of sorbent is mixed into reaction kettle, after mixing evenly, is staticly settled；
(5) liquid in step (4) was pumped into millipore filter and was filtered, the impurity for filtering out adsorbent and absorption turns
It send to crystallization kettle, and nitrogen filled protection is carried out to crystallization kettle；
(6) it is passed through circulating water cooling in crystallization kettle collet, when temperature is down to 30 DEG C, opens the bottom valve of crystallization kettle, it will
Material in crystallization kettle, which is put into suction filtration tank, to be drained, and brilliant solid 4,4 '-diaminodiphenyl ether is obtained；
(7) solid 4, the 4 '-diaminodiphenyl ether of crystalline substance in step (6) is put into a centrifuge, and added into centrifuge
Enter water, after stirring 15min, then carries out centrifugal treating；
(8) it in the filter cake investment vacuum drier for obtaining step (7) centrifugation, is dried to get 4,4 '-diaminos
Yl diphenyl ether.
Wherein, the mixed solvent in the step (1) is formulated by methanol and dimethyl acetamide in the ratio of 1:1.4
's.
Wherein, the multiple evacuation note nitrogen in the step (1) is to vacuumize six times, is added nitrogen five times, and guarantee to vacuumize
When dissolution kettle collet heating be no more than 25 DEG C.
Wherein, the filter sizes of the millipore filter in the step (5) are 0.3-0.8 μm.
Wherein, the recirculated water flow velocity in the step (6) is 1.4L/min.
Wherein, vacuum drying condition in the step (8) are as follows: vacuum degree -0.08Mpa, 86 DEG C of drying temperature, when dry
Between 50min.
Obtained above 4,4 '-diaminodiphenyl ethers are detected into its purity, purity 99.97% with gas chromatography.
Embodiment 4
The method of 4, the 4 '-diaminodiphenyl ether secondary crystallization of production of the present embodiment, comprising the following steps:
(1) 1270kg mixed solvent is put into dissolution kettle, puts into 300kg block 4 into reaction kettle while stirring,
4 '-diaminodiphenyl ethers close the valve that feeds intake, and carry out repeatedly evacuating note nitrogen to closed dissolution kettle, to form airfree bear
Press nitrogen environment；
(2) lead to steam to dissolution kettle collet, be heated to 58 DEG C, continue to stir 42min, 4,4 '-diamino two of block
Phenylate all dissolves；
(3) liquid in the dissolution kettle of step (2) is pumped into filter press and is filtered, and filtrate is transferred in reaction kettle；
(4) activated carbon of sorbent is mixed into reaction kettle, after mixing evenly, is staticly settled；
(5) liquid in step (4) was pumped into millipore filter and was filtered, the impurity for filtering out adsorbent and absorption turns
It send to crystallization kettle, and nitrogen filled protection is carried out to crystallization kettle；
(6) it is passed through circulating water cooling in crystallization kettle collet, when temperature is down to 28 DEG C, opens the bottom valve of crystallization kettle, it will
Material in crystallization kettle, which is put into suction filtration tank, to be drained, and brilliant solid 4,4 '-diaminodiphenyl ether is obtained；
(7) solid 4, the 4 '-diaminodiphenyl ether of crystalline substance in step (6) is put into a centrifuge, and added into centrifuge
Enter water, after stirring 13min, then carries out centrifugal treating；
(8) it in the filter cake investment vacuum drier for obtaining step (7) centrifugation, is dried to get 4,4 '-diaminos
Yl diphenyl ether.
Wherein, the mixed solvent in the step (1) is formulated by methanol and dimethyl acetamide in the ratio of 1:1.3
's.
Wherein, the multiple evacuation note nitrogen in the step (1) is to vacuumize six times, is added nitrogen five times, and guarantee to vacuumize
When dissolution kettle collet heating be no more than 25 DEG C.
Wherein, the filter sizes of the millipore filter in the step (5) are 0.3-0.8 μm.
Wherein, the recirculated water flow velocity in the step (6) is 1.3L/min.
Wherein, vacuum drying condition in the step (8) are as follows: vacuum degree -0.07Mpa, 85 DEG C of drying temperature, when dry
Between 45min.
Obtained above 4,4 '-diaminodiphenyl ethers are detected into its purity, purity 99.95% with gas chromatography.
Embodiment 5
The method of 4, the 4 '-diaminodiphenyl ether secondary crystallization of production of the present embodiment, comprising the following steps:
(1) 1320kg mixed solvent is put into dissolution kettle, puts into 300kg block 4 into reaction kettle while stirring,
4 '-diaminodiphenyl ethers close the valve that feeds intake, and carry out repeatedly evacuating note nitrogen to closed dissolution kettle, to form airfree bear
Press nitrogen environment；
(2) lead to steam to dissolution kettle collet, be heated to 62 DEG C, continue to stir 48min, 4,4 '-diamino two of block
Phenylate all dissolves；
(3) liquid in the dissolution kettle of step (2) is pumped into filter press and is filtered, and filtrate is transferred in reaction kettle；
(4) activated carbon of sorbent is mixed into reaction kettle, after mixing evenly, is staticly settled；
(5) liquid in step (4) was pumped into millipore filter and was filtered, the impurity for filtering out adsorbent and absorption turns
It send to crystallization kettle, and nitrogen filled protection is carried out to crystallization kettle；
(6) it is passed through circulating water cooling in crystallization kettle collet, when temperature is down to 32 DEG C, opens the bottom valve of crystallization kettle, it will
Material in crystallization kettle, which is put into suction filtration tank, to be drained, and brilliant solid 4,4 '-diaminodiphenyl ether is obtained；
(7) solid 4, the 4 '-diaminodiphenyl ether of crystalline substance in step (6) is put into a centrifuge, and added into centrifuge
Enter water, after stirring 18min, then carries out centrifugal treating；
(8) it in the filter cake investment vacuum drier for obtaining step (7) centrifugation, is dried to get 4,4 '-diaminos
Yl diphenyl ether.
Wherein, the mixed solvent in the step (1) is formulated by methanol and dimethyl acetamide in the ratio of 1:1.5
's.
Wherein, the multiple evacuation note nitrogen in the step (1) is to vacuumize six times, is added nitrogen five times, and guarantee to vacuumize
When dissolution kettle collet heating be no more than 25 DEG C.
Wherein, the filter sizes of the millipore filter in the step (5) are 0.3-0.8 μm.
Wherein, the recirculated water flow velocity in the step (6) is 1.5L/min.
Wherein, vacuum drying condition in the step (8) are as follows: vacuum degree -0.05Mpa, 86 DEG C of drying temperature, when dry
Between 55min.
Obtained above 4,4 '-diaminodiphenyl ethers are detected into its purity, purity 99.93% with gas chromatography.
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. a kind of method for producing 4,4'- diaminodiphenyl ether secondary crystallization, which comprises the following steps:
(1) mixed solvent is put into dissolution kettle, while stirring the investment block 4 into reaction kettle, 4'- diaminodiphenyl ether,
The weight ratio of the block 4 of investment, 4'- diaminodiphenyl ether and mixed solvent is 1:4.2-4.5, the valve that feeds intake is closed, to closing
Dissolution kettle carry out repeatedly evacuate note nitrogen, to form airfree negative pressure nitrogen environment；
(2) lead to steam to dissolution kettle collet, be heated to 55-65 DEG C, continue to stir 40-50min, block 4,4'- diamino
Diphenyl ether all dissolves；
(3) liquid in the dissolution kettle of step (2) is pumped into filter press and is filtered, and filtrate is transferred in reaction kettle；
(4) activated carbon of sorbent is mixed into reaction kettle, after mixing evenly, is staticly settled；
(5) liquid in step (4) was pumped into millipore filter and was filtered, the impurity for filtering out adsorbent and absorption transfers to
Crystallization kettle, and nitrogen filled protection is carried out to crystallization kettle；
(6) it is passed through circulating water cooling in crystallization kettle collet, when temperature is down to 25-35 DEG C, opens the bottom valve of crystallization kettle, will ties
Material in brilliant kettle, which is put into suction filtration tank, to be drained, and brilliant solid 4,4'- diaminodiphenyl ether is obtained；
(7) solid 4, the 4'- diaminodiphenyl ether of crystalline substance in step (6) is put into a centrifuge, and water is added into centrifuge,
After stirring 10-20min, then carry out centrifugal treating；
(8) it in the filter cake investment vacuum drier for obtaining step (7) centrifugation, is dried to get 4,4'- diamino two
Phenylate.
2. the method for production 4,4'- diaminodiphenyl ether secondary crystallization according to claim 1, which is characterized in that described
What the mixed solvent in step (1) was formulated by methanol and dimethyl acetamide in the ratio of 1:1.2-1.6.
3. the method for production 4,4'- diaminodiphenyl ether secondary crystallization according to claim 1, which is characterized in that described
Multiple evacuation note nitrogen in step (1) is to vacuumize six times, and dissolution kettle collet heats not when adding nitrogen five times, and guaranteeing to vacuumize
More than 25 DEG C.
4. the method for production 4,4'- diaminodiphenyl ether secondary crystallization according to claim 1, which is characterized in that described
In step (2), lead to steam to dissolution kettle collet, be heated to 60 DEG C, continues to stir 45min, block 4,4'- diamino hexichol
Ether all dissolves.
5. the method for production 4,4'- diaminodiphenyl ether secondary crystallization according to claim 1, which is characterized in that described
The filter sizes of millipore filter in step (5) are 0.3-0.8 μm.
6. the method for production 4,4'- diaminodiphenyl ether secondary crystallization according to claim 1, which is characterized in that described
Recirculated water flow velocity in step (6) is 1.2-1.6L/min.
7. the method for production 4,4'- diaminodiphenyl ether secondary crystallization according to claim 1, which is characterized in that described
Vacuum drying condition in step (8) are as follows: vacuum degree≤- 0.09Mpa, 84-88 DEG C of drying temperature, drying time 40-60min.
8. the method for production 4,4'- diaminodiphenyl ether secondary crystallization according to claim 7, which is characterized in that described
Vacuum drying condition in step (8) are as follows: vacuum degree -0.08Mpa, 86 DEG C of drying temperature, drying time 50min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112341345A (en) * | 2020-08-19 | 2021-02-09 | 山东欧亚化工有限公司 | Method and system for extracting 4,4' -diaminodiphenyl ether from DMAC (dimethylacetamide) medium |
| CN115010612A (en) * | 2022-06-24 | 2022-09-06 | 河北海力香料股份有限公司 | Crystallization process of 4,4' -diaminodiphenyl ether |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107353214A (en) * | 2017-07-13 | 2017-11-17 | 山东冠森高分子材料科技股份有限公司 | With the directly refined 4,4 ＇ diaminodiphenyl ether techniques of mixed solvent recrystallization |
| CN108752222A (en) * | 2018-08-20 | 2018-11-06 | 万达集团股份有限公司 | A kind of the crystallization and purification technique and crystallization and purification system of 4,4 '-diaminodiphenyl ethers |
| CN109180504A (en) * | 2018-08-20 | 2019-01-11 | 万达集团股份有限公司 | A kind of recovery and treatment method of 4,4`- diaminodiphenyl ether distillation residue |
-
2019
- 2019-04-26 CN CN201910344817.3A patent/CN110015965A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107353214A (en) * | 2017-07-13 | 2017-11-17 | 山东冠森高分子材料科技股份有限公司 | With the directly refined 4,4 ＇ diaminodiphenyl ether techniques of mixed solvent recrystallization |
| CN108752222A (en) * | 2018-08-20 | 2018-11-06 | 万达集团股份有限公司 | A kind of the crystallization and purification technique and crystallization and purification system of 4,4 '-diaminodiphenyl ethers |
| CN109180504A (en) * | 2018-08-20 | 2019-01-11 | 万达集团股份有限公司 | A kind of recovery and treatment method of 4,4`- diaminodiphenyl ether distillation residue |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112341345A (en) * | 2020-08-19 | 2021-02-09 | 山东欧亚化工有限公司 | Method and system for extracting 4,4' -diaminodiphenyl ether from DMAC (dimethylacetamide) medium |
| CN115010612A (en) * | 2022-06-24 | 2022-09-06 | 河北海力香料股份有限公司 | Crystallization process of 4,4' -diaminodiphenyl ether |
| CN115010612B (en) * | 2022-06-24 | 2023-08-15 | 河北海力恒远新材料股份有限公司 | Crystallization process of 4,4' -diaminodiphenyl ether |
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