CN107619367A - A kind of method that crystallisation by cooling method improves bisphenol AF whiteness - Google Patents
A kind of method that crystallisation by cooling method improves bisphenol AF whiteness Download PDFInfo
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- CN107619367A CN107619367A CN201710824980.0A CN201710824980A CN107619367A CN 107619367 A CN107619367 A CN 107619367A CN 201710824980 A CN201710824980 A CN 201710824980A CN 107619367 A CN107619367 A CN 107619367A
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Abstract
The present invention relates to chemical field, discloses a kind of method that crystallisation by cooling method improves bisphenol AF whiteness, including：1）Add absolute methanol, bisphenol AF crude product and atlapulgite, activated carbon, hydrogen peroxide or tartaric acid successively into reactor, be stirred；2）Heating, by reactor temperature control at 63 67 DEG C, the 70min of aging 50；3）After bisphenol AF crude product is completely dissolved, first Temperature fall goes out crystalline substance to 50 54 DEG C, the 35min of growing the grain 25, is cooled to 8 12 DEG C；4）By gained crystallization filtering, elution, dry；5）Repeat crystallisation by cooling once, finished product.Present invention finds multiple influence factors to bisphenol AF whiteness with material impact undiscovered so far in the prior art, and the method that have developed the raising bisphenol AF product whiteness of a set of completion based on this, experimental result shows that the inventive method can effectively improve the whiteness of bisphenol AF.
Description
Technical field
The present invention relates to chemical field, more particularly to a kind of method that crystallisation by cooling method improves bisphenol AF whiteness.
Background technology
The crosslinking agent for being mainly used as fluorine class rubber of bisphenol AF, it can make rubber that there is good resistance to compression compression deformation, resist
Chemical attack and heat endurance.Bisphenol AF can synthesize special fluorinated polyimide, fluorine-containing polyamide, fluorine-containing poly- as monomer
Ester, fluorine-containing makrolon and other fluoropolymers, as gas separation membrane, dielectric coating, optical fiber jacket, photoelectric tube base material,
Binding agent etc., it is widely used in microelectronics, optics, space technology etc..
At present, the preparation method of bisphenol AF is a lot, as Chinese patent CN200810243703.1 discloses a kind of bisphenol AF
Preparation method, first by catalyst, aniline and HFA3H2O is added separately in reactor, after back flow reaction, is added organic
Solvent, intermediate 1 is obtained after dissolving, filter, rotate；Secondly, intermediate obtained by natrium nitrosum and the first step is added into sulfuric acid
1, after diazo-reaction, mixed liquor is gone into hydrolysis in sulfuric acid, then through extracting, wash, except solvent after intermediate 2；Most
Afterwards, intermediate 2 and phenol obtained by catalyst, second step are added in reactor respectively, back flow reaction, then extracted through organic solvent
Take, wash, except after solvent bisphenol AF.But obtained bisphenol AF in the prior art, generally turn to be yellow, whiteness is not ideal enough, shadow
Product quality is rung.Therefore the whiteness of bisphenol AF how is simply and effectively improved, is the technical problem of urgent need to resolve.
The content of the invention
In order to solve the above-mentioned technical problem, the invention provides a kind of crystallisation by cooling method improve bisphenol AF whiteness method,
The inventive method can effectively improve the whiteness of bisphenol AF.
The present invention concrete technical scheme be：A kind of method that crystallisation by cooling method improves bisphenol AF whiteness, including following step
Suddenly：1) absolute methanol, the bisphenol AF crude product of 1100-1300 parts by weight of 2000-2800 parts by weight are added successively into reactor
Atlapulgite, activated carbon, hydrogen peroxide or tartaric acid with 10-14 parts by weight, are stirred.
Atlapulgite, activated carbon, hydrogen peroxide or tartaric acid are added in a solvent.Wherein, activated carbon, atlapulgite can be inhaled
Attached impurity, crystallization whiteness is improved, hydrogen peroxide has strong oxidizing property, by oxidative decoloration, improves whiteness.And the effect of tartaric acid is
Whiteness is improved by antioxidation.
2) heat up, by reactor temperature control at 63-67 DEG C, aging 50-70min.
3) after bisphenol AF crude product is completely dissolved, first Temperature fall goes out crystalline substance to 50-54 DEG C, growing the grain 25-35min, opens reaction
The chilled brine imported valve of kettle, is cooled to 8-12 DEG C.
4) gained crystallization is filtered, eluted, dried.
5) repeat step 1) to step 4) crystallisation by cooling once, finished product.
The inventors discovered that during using crystallisation by cooling method, crystallization is carried out to repeat crystallization once, and strictly control second
Speed during secondary crystallization cooling, the whiteness of final products can be greatly improved.
Preferably, in step 1), stir speed (S.S.) 450-550r/min.
The inventors discovered that rotating speed increase can reduce granularity, and the present inventor has found, particle diameter is influence product whiteness
Most important factor, particle diameter is smaller, and whiteness is relatively better, therefore rotating speed should try one's best increase, but needs control limit, rotating speed mistake
Conference causes liquid to be stained with crystallizer wall.
Preferably, in step 1), addition for tartaric acid.
In above-mentioned various reagents, hydrogen peroxide is with can pass through oxidative decoloration；But phenols can be oxidized to quinone simultaneously.It is living
Property charcoal and activated decoloration, there is certain decolorizing effect but unobvious in practical operation；And filtering trouble, easily by activated carbon
Bring into, cause product quality unqualified.And tartaric acid can not only be decolourized by antioxidation, and its faintly acid also just can
Ensure that phenols is not oxidized into quinone (bisphenol AF can change colour under the conditions of weak base).
Preferably, in step 3), rate of temperature fall is 13-17 DEG C/h.
Preferably, in step 4), first crystallization is eluted with absolute methanol, then crystallization washed with water.
After being eluted to the product of filtering, it is possible to increase whiteness.The surface of product can incite somebody to action when being filtered with eluent solvent
Product surface yellow is washed off.
The inventors discovered that different elution techniques also have considerable influence to product whiteness, therefore devise three kinds of elution sides
Method：1. filtering product first with eluent solvent and then is washed with water；2. dry product is washed with water；3. filtering product is directly used
Water washing.By it was found that, 1. method has best effect.
Preferably, in step 5), in the step 3) of second of crystallisation by cooling, rate of temperature fall is 1-3 DEG C/h.
The inventors discovered that during using crystallisation by cooling method, crystallization is carried out to repeat crystallization once, and strictly control second
Speed during secondary crystallization cooling, the whiteness of final products can be greatly improved.
It is compared with the prior art, the beneficial effects of the invention are as follows：Do not sent out so far in the prior art present invention finds multiple
The existing influence factor to bisphenol AF whiteness with material impact, and the raising bis-phenol of a set of completion is have developed based on this
The method of AF product whiteness, practice result show that the inventive method can effectively improve the whiteness of bisphenol AF.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of method that crystallisation by cooling method improves bisphenol AF whiteness, comprises the following steps：
1) absolute methanol of 2400 parts by weight, the bisphenol AF crude product of 1200 parts by weight and 12 parts by weight are added successively into reactor
Tartaric acid, be stirred (stir speed (S.S.) 500r/min).
2) heat up, by reactor temperature control at 65 DEG C, aging 60min.
3) after bisphenol AF crude product is completely dissolved, first Temperature fall goes out crystalline substance to 52 DEG C, growing the grain 30min, opens the cold of reactor
Freeze brine inlet valve, be cooled to 10 DEG C, rate of temperature fall is 15 DEG C/h.
4) gained crystallization is filtered, eluted, dried.Wherein, first crystallization is eluted with absolute methanol, then with water to knot
Crystalline substance is washed.
5) repeat step 1) to step 4) crystallisation by cooling once, finished product.Wherein, the step 3) of second of crystallisation by cooling
In, rate of temperature fall is 2 DEG C/h.
Embodiment 2
A kind of method that crystallisation by cooling method improves bisphenol AF whiteness, comprises the following steps：
1) absolute methanol of 2000 parts by weight, the bisphenol AF crude product of 1100 parts by weight and 10 parts by weight are added successively into reactor
Tartaric acid, be stirred (stir speed (S.S.) 450r/min).
2) heat up, by reactor temperature control at 63 DEG C, aging 70min.
3) after bisphenol AF crude product is completely dissolved, first Temperature fall goes out crystalline substance to 50 DEG C, growing the grain 35min, opens the cold of reactor
Freeze brine inlet valve, be cooled to 8 DEG C, rate of temperature fall is 13 DEG C/h.
4) gained crystallization is filtered, eluted, dried.Wherein, first crystallization is eluted with absolute methanol, then with water to knot
Crystalline substance is washed.
5) repeat step 1) to step 4) crystallisation by cooling once, finished product.Wherein, the step 3) of second of crystallisation by cooling
In, rate of temperature fall is 1 DEG C/h.
Embodiment 3
A kind of method that crystallisation by cooling method improves bisphenol AF whiteness, comprises the following steps：
1) absolute methanol of 2800 parts by weight, the bisphenol AF crude product of 1300 parts by weight and 14 parts by weight are added successively into reactor
Tartaric acid, be stirred (stir speed (S.S.) 550r/min).
2) heat up, by reactor temperature control at 67 DEG C, aging 50min.
3) after bisphenol AF crude product is completely dissolved, first Temperature fall goes out crystalline substance to 54 DEG C, growing the grain 25min, opens the cold of reactor
Freeze brine inlet valve, be cooled to 12 DEG C, rate of temperature fall is 17 DEG C/h.
4) gained crystallization is filtered, eluted, dried.Wherein, first crystallization is eluted with absolute methanol, then with water to knot
Crystalline substance is washed.
5) repeat step 1) to step 4) crystallisation by cooling once, finished product.Wherein, the step 3) of second of crystallisation by cooling
In, rate of temperature fall is 3 DEG C/h.
Embodiment 4
A kind of method that crystallisation by cooling method improves bisphenol AF whiteness, comprises the following steps：
1) absolute methanol of 2400 parts by weight, the bisphenol AF crude product of 1200 parts by weight and 10-14 weights are added successively into reactor
The atlapulgite of part is measured, is stirred (stir speed (S.S.) 500r/min).
2) heat up, by reactor temperature control at 65 DEG C, aging 60min.
3) after bisphenol AF crude product is completely dissolved, first Temperature fall goes out crystalline substance to 52 DEG C, growing the grain 30min, opens the cold of reactor
Freeze brine inlet valve, be cooled to 10 DEG C, rate of temperature fall is 15 DEG C/h.
4) gained crystallization is filtered, eluted, dried.Wherein, first crystallization is eluted with absolute methanol, then with water to knot
Crystalline substance is washed.
5) repeat step 1) to step 4) crystallisation by cooling once, finished product.Wherein, the step 3) of second of crystallisation by cooling
In, rate of temperature fall is 2 DEG C/h.
Embodiment 5
A kind of method that crystallisation by cooling method improves bisphenol AF whiteness, comprises the following steps：
1) absolute methanol of 2400 parts by weight, the bisphenol AF crude product of 1200 parts by weight and 10-14 weights are added successively into reactor
The activated carbon of part is measured, is stirred (stir speed (S.S.) 500r/min).
2) heat up, by reactor temperature control at 65 DEG C, aging 60min.
3) after bisphenol AF crude product is completely dissolved, first Temperature fall goes out crystalline substance to 52 DEG C, growing the grain 30min, opens the cold of reactor
Freeze brine inlet valve, be cooled to 10 DEG C, rate of temperature fall is 15 DEG C/h.
4) gained crystallization is filtered, eluted, dried.Wherein, first crystallization is eluted with absolute methanol, then with water to knot
Crystalline substance is washed.
5) repeat step 1) to step 4) crystallisation by cooling once, finished product.Wherein, the step 3) of second of crystallisation by cooling
In, rate of temperature fall is 2 DEG C/h.
Embodiment 6
A kind of method that crystallisation by cooling method improves bisphenol AF whiteness, comprises the following steps：
1) absolute methanol of 2400 parts by weight, the bisphenol AF crude product of 1200 parts by weight and 10-14 weights are added successively into reactor
The hydrogen peroxide of part is measured, is stirred (stir speed (S.S.) 500r/min).
2) heat up, by reactor temperature control at 65 DEG C, aging 60min.
3) after bisphenol AF crude product is completely dissolved, first Temperature fall goes out crystalline substance to 52 DEG C, growing the grain 30min, opens the cold of reactor
Freeze brine inlet valve, be cooled to 10 DEG C, rate of temperature fall is 15 DEG C/h.
4) gained crystallization is filtered, eluted, dried.Wherein, first crystallization is eluted with absolute methanol, then with water to knot
Crystalline substance is washed.
5) repeat step 1) to step 4) crystallisation by cooling once, finished product.Wherein, the step 3) of second of crystallisation by cooling
In, rate of temperature fall is 2 DEG C/h.
Whiteness detects
Whiteness detection is carried out to finished product made from embodiment 1, embodiment 4-6, it is as a result as follows：
From the foregoing, it will be observed that after being added with tartaric acid, atlapulgite, activated carbon and hydrogen peroxide, the whiteness of crystallization can be effectively improved, and
And add tartarated best results, and compared with hydrogen peroxide, phenols will not be oxidized to quinones.
Raw materials used in the present invention, equipment, it is the conventional raw material, equipment of this area unless otherwise noted；In the present invention
Method therefor, it is the conventional method of this area unless otherwise noted.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions, it is every according to the present invention
Any simple modification, change and the equivalent transformation that technical spirit is made to above example, still fall within the technology of the present invention side
The protection domain of case.
Claims (6)
1. a kind of method that crystallisation by cooling method improves bisphenol AF whiteness, it is characterised in that comprise the following steps：
1）Add absolute methanol, the bisphenol AF crude product of 1100-1300 parts by weight of 2000-2800 parts by weight successively into reactor
Atlapulgite, activated carbon, hydrogen peroxide or tartaric acid with 10-14 parts by weight, are stirred；
2）Heating, by reactor temperature control at 63-67 DEG C, aging 50-70min；
3）After bisphenol AF crude product is completely dissolved, first Temperature fall goes out crystalline substance to 50-54 DEG C, growing the grain 25-35min, opens reactor
Chilled brine imported valve, is cooled to 8-12 DEG C；
4）By gained crystallization filtering, elution, dry；
5）Repeat step 1）To step 4）Crystallisation by cooling once, finished product.
2. the method that a kind of crystallisation by cooling method as claimed in claim 1 improves bisphenol AF whiteness, it is characterised in that step 1）
In, stir speed (S.S.) 450-550r/min.
3. the method that a kind of crystallisation by cooling method as claimed in claim 1 or 2 improves bisphenol AF whiteness, it is characterised in that step
1）In, addition for tartaric acid.
4. the method that a kind of crystallisation by cooling method as claimed in claim 1 improves bisphenol AF whiteness, it is characterised in that step 3）
In, rate of temperature fall is 13-17 DEG C/h.
5. the method that a kind of crystallisation by cooling method as claimed in claim 1 improves bisphenol AF whiteness, it is characterised in that step 4）
In, first crystallization is eluted with absolute methanol, then crystallization is washed with water.
6. the method that a kind of crystallisation by cooling method as claimed in claim 1 improves bisphenol AF whiteness, it is characterised in that step 5）
In, the step 3 of second of crystallisation by cooling）In, rate of temperature fall is 1-3 DEG C/h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710824980.0A CN107619367B (en) | 2017-09-13 | 2017-09-13 | Method for improving whiteness of bisphenol AF (Acrylonitrile-butadiene-styrene) by cooling crystallization method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710824980.0A CN107619367B (en) | 2017-09-13 | 2017-09-13 | Method for improving whiteness of bisphenol AF (Acrylonitrile-butadiene-styrene) by cooling crystallization method |
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| CN107619367A true CN107619367A (en) | 2018-01-23 |
| CN107619367B CN107619367B (en) | 2020-05-12 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06145090A (en) * | 1992-11-02 | 1994-05-24 | Honsyu Kagaku Kogyo Kk | Bisphenol af excellent in optical property and its production |
| CN1907951A (en) * | 2006-08-18 | 2007-02-07 | 上海化学试剂研究所 | Purifying method of 2,2-di(3-amido-4-hydroxyphenyl)hexafluoropropane |
| CN105753710A (en) * | 2014-12-18 | 2016-07-13 | 连云港市泰卓新材料有限公司 | Environmentally friendly preparation technology of 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane |
-
2017
- 2017-09-13 CN CN201710824980.0A patent/CN107619367B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06145090A (en) * | 1992-11-02 | 1994-05-24 | Honsyu Kagaku Kogyo Kk | Bisphenol af excellent in optical property and its production |
| CN1907951A (en) * | 2006-08-18 | 2007-02-07 | 上海化学试剂研究所 | Purifying method of 2,2-di(3-amido-4-hydroxyphenyl)hexafluoropropane |
| CN105753710A (en) * | 2014-12-18 | 2016-07-13 | 连云港市泰卓新材料有限公司 | Environmentally friendly preparation technology of 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane |
Non-Patent Citations (1)
| Title |
|---|
| 张亨: "双酚AF的合成研究进展", 《有机氟工业》 * |
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Denomination of invention: A cooling crystallization method to improve the whiteness of bisphenol AF Effective date of registration: 20201223 Granted publication date: 20200512 Pledgee: Zhejiang Jiangshan rural commercial bank Limited by Share Ltd. Pledgor: ZHEJIANG HILL CHEMICAL Co.,Ltd. Registration number: Y2020330001267 |