CN109928944A - A kind of preparation method of 4,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids - Google Patents
A kind of preparation method of 4,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids Download PDFInfo
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- CN109928944A CN109928944A CN201910256023.1A CN201910256023A CN109928944A CN 109928944 A CN109928944 A CN 109928944A CN 201910256023 A CN201910256023 A CN 201910256023A CN 109928944 A CN109928944 A CN 109928944A
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Abstract
The present invention relates to field of material preparation, specially a kind of preparation method of 4,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acid acid anhydrides.Method includes the following steps: first by granular 4,4'- (hexafluoro isopropenyl)-two ortho-xylenes in the nano-milled dispersion machine of wet type with water grinding dispersion.Then 4 after dispersion, 4'- (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) and aqueous hydrogen peroxide solution are separately added into evenly dispersed in Photoreactor, then under reaction temperature appropriate, open the cold ultraviolet light of LED, UV light-induced light source irradiation reaction solution reacts certain time, then it reheats oxidation reaction after the completion to filter reaction solution, filters obtain 6-FTA after cooling.6-FTA is finally put into drying and dewatering in microwave vacuum baking oven and obtains 6-FDA product.This method preparation process is simple, environmentally protective, and it is extremely low to prepare product yield high, purity is high and metal ion content, facilitates industrialized production.
Description
Technical field
The present invention relates to technical field of material, specially a kind of system of 4,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acid acid anhydrides
Preparation Method.
Background technique
4,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acid acid anhydrides (6FDA) are a kind of new type polyimide monomer materials, use hexafluoro
Polyimides of the dianhydride as monomer, mainly there is following advantage: 1) low-k in performance.Jie of common polyimides
For electric constant 3.4 or so, and after 6FDA is added, dielectric constant can be reduced to 2.5.Low-k bring is signal delay
With the reduction of loss, this has very big value in electrical applications.2) transparency and controllable refractive index.Because polyimides is
Slightly yellowish or brown, after 6FDA is added, can so that it becomes transparent, and according to 6FDA be added how much, can control its folding
It penetrates rate (refractive index), these performances play the role of very big in optical element application.3) chemistry and thermostabilization
Property.After introducing fluorine atom, because of the strong elecrtonegativity of fluorine atom, the chemistry and thermal stability of polyimides can be improved.So that product
Can special chemistry or at a temperature of work.4) lubricity.Because of the low polarity of fluorine atom, so that fluorinated polyamides is sub-
Amine has very low surface free energy, and surface is smooth, and frictional force is small.5) have very with the fluorinated polyimide material that 6FDA is synthesized
Good resistance to thermooxidation, high temperature hot melt and radiation hardness, is the structural material of aerospace industry first choice.
6-FDA synthetic route mainly includes that three steps: the first step, Hexafluoro acetone and dimethylbenzene are alkylated under acid catalysis
Reaction obtains compound 4,4'- (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP)；Second step, 6- FXP is under certain condition
It is oxidized to 4,4'- (hexafluoro isopropyl alkene) two phthalandiones (6-FTA)；Third step, 6-FTA generate final product 6- through dehydration
FDA.Wherein second step is committed step, and the purity of the yield of 6-FTA directly affects the quality of final product 6-FDA, reaction
Equation is as follows:
The current oxidation process includes dilute HNO3KMnO under method, alkaline condition4Method and transition metal-catalyzed air oxidation process work
Skill.United States Patent (USP) US3356648 discloses HNO in a kind of autoclave3Method prepares 6- FTA, and crude product yield is only 83.6%,
Reaction generates a large amount of NOx, environmental pollution is caused, pressure rise is also resulted in, increases danger coefficient.Patent US20090156834
Improve dilute HNO3Method oxidation technology, use it is micro- it is counter be nitric acid continuous oxidation method, the nitrogen-containing oxide generated after reaction is into one
It walks reuse and generates HNO3, realize its reuse, yield can reach 97%.Although the yield of continuous reaction method compares batch process
It is good, but its reaction temperature high (200 DEG C or more), reaction pressure are big (4MPa), and safely and effectively production cannot ensure.Dilute HNO3
Method has the disadvantage in that (1) HNO3Consumption is big, is at least 7 or more with the molar ratio of raw material；(2) corrosive equipment；(3) by
High temperature and high pressure is needed in reaction, especially in HNO3Under the conditions of existing, operational hazards.
Zhu etc. (Journal of Fluorine Chemistry, 2003,123,221-225) is reported in alkaline condition
Under use KMnO4Oxidation 6-FXP obtains target product 6-FTA, yield 66%.Chinese patent CN101696199A is disclosed with first
Benzene/water is as using KMnO under mixed solvent4The yield of oxidized compound 6- FXP, 6-FTA can reach 70%, and operating procedure is multiple
Miscellaneous, solvent usage is larger.KMnO4The product yield that method obtains is low, and purity is not high, and separating step is cumbersome, and hygroscopicity is stronger,
In addition KMnO4Method consumes a large amount of oxidants, generates a large amount of rufous liquid waste liquid and solid by-product needs to handle, in product
Metal ion be difficult to separate.
Transition metal ion catalyst oxidizing process is the Catalytic processes using oxygen as oxidant.1991, US5004797,
The patents such as US4987238 and DE3739800A1 disclose the side a metal ion species-Br-system oxygen catalytic oxidation 6-FTA
Method, yield are up to 88.4%.Patent US5194633 uses similar reaction process, and the yield of 6-FDA reaches 91%；Japan
Patent JP2002097185 also discloses using Co, Mn, Ce and different Br-source catalytic air oxidation 6-FXP technique,
The yield of 6-FTA reaches 96.0%, purity 98.6%.Patent CN105061186B utilizes 4,4'- (hexafluoro isopropenyl)-two
For ortho-xylene in the presence of-Br-co-catalyst, metal ion Co is added in distribution2+、Mn2+、Ce2+、Fe2+Equal catalytic oxygens carry out oxygen
Change reaction preparation 4,4'- hexafluoro isopropyl alkene) two phthalandiones, compared to the dosage that above-mentioned patent reduces metal ion catalyst, so that
6-FTA highest yield reaches 96%, purity 97%.But to reach higher reaction selectivity, the parameter in reaction process needs
Accurate to adjust control, current main method is setting stepwise reaction temperature, the journey of the temperature control oxidation by adjusting reaction
Degree, this method are unfavorable for the stability of reaction process.In addition, since reaction generates in ortho position carboxyl and the reaction system of product
Metal ion catalyst salt easily generated and reduce the activity of catalyst, so the dosage of metal ion catalyst is larger, increase
Reaction cost and isolated difficulty.
Summary of the invention
It is an object of the invention to propose one kind 4 for disadvantage and problem of the existing technology in background technique,
The preparation method of 4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids.This method is a kind of completely new scheme, and it is low to solve product yield, pure
Degree is not high, and reaction step is cumbersome, and hygroscopicity is stronger, and reaction process energy consumption is high, the separation of reaction process metal ion difficulty, solvent
The problems such as dosage is big, and high-temperature high-voltage reaction is dangerous.
In order to realize the above goal of the invention, the technical scheme of the invention to solve the technical problem is:
A kind of preparation method of 4,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids comprising following steps:
A, first by granular 4,4'- (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) at nano-milled point of wet type
Dissipate machine in water grinding dispersion.
B, then-two ortho-xylene (6- of nanoscale 4,4'- (hexafluoro isopropenyl) after a certain proportion of dispersion
FXP) and aqueous hydrogen peroxide solution be separately added into it is evenly dispersed in Photoreactor, then under reaction temperature appropriate, open LED it is cold
Ultraviolet light, UV light-induced light source irradiation reaction solution react certain time, then reheat oxidation reaction after the completion for reaction solution
Filtering filters obtain 6-FTA after cooling.
C, 6-FTA is finally put into drying and dewatering in microwave vacuum baking oven and obtains 6-FDA product.
The nanometer wet process disintegrator, 0.08~20KW of power, the weight of smashing fineness 10~100nm, 6-FXP and water
Than are as follows: 100::20~200, so that smashed 6-FXP and aqueous solution moment uniform dispersion and emulsion, still divide after for 24 hours
It dissipates uniform.
The uv induction oxidation reaction mechanism and process include: that hydrogen peroxide first absorbs luminous energy under ultraviolet light
Afterwards, so that O -- O bond fracture generates strong oxidizing property OH hydroxyl free radical and oxygen atom.H2O2Ultraviolet photolysis following reaction occurs:
H2O2+hv→2·OH
·OH+H2O2→H2O+·HO2
·HO2+H2O2→H2O+·OH+O2
Because the OH hydroxyl free radical generated has strong oxidizing property, while 6-FXP molecule can quilt under ultraviolet light
Promoting vibration excited state, OH hydroxyl free radical and dissolved oxygen and the methyl of organic compound 6-FXP can be oxidized to first
Aldehyde radical continues to be oxidized reaction to be carboxyl.
Chemical equation is as follows:
The mass concentration of the aqueous hydrogen peroxide solution is 50%~80%, 4,4'- (hexafluoro isopropenyl)-two neighbours two
The mass ratio of toluene (6-FXP) dispersion liquid and aqueous hydrogen peroxide solution is 100:48~192.
The reaction temperature is -6~32 DEG C, and reaction pressure is normal pressure, after reacting 1.2~2.5h, is heated to 50~60
DEG C, react 2.4~12h.The optimal conditions of reaction are as follows: 55 DEG C of reaction 4.2h are heated to after 10 DEG C of synthesis under normal pressure 2h.
The cold ultraviolet light is long wave ultraviolet light lamp, and wavelength 320-400nm, power is 0.1~20KW, and most optimum wavelengths are
380nm。
The filter device is nano-film filtration device, aperture 12nm.
The microwave vacuum baking oven, microwave frequency 2.45GHz ± 25MHz, 1~50KW of power is adjustable, and dewatering time 0.2~
3h。
Reached using 4,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acid yields that the best techniques indicator conditions are prepared
98.1%, purity 99.937%, metal ion reaches 0.01ppm rank.
Compared with the prior art, the advantages of the present invention are as follows:
(1), UV light-induced chemical reaction is the Fast Process of a kind of orientation, low reaction activation energy, with height
Selectivity, therefore the generation of reaction time and by-product is greatly reduced, it is significantly high compared with traditional handicraft yield and purity.
(2), oxidation reaction is easy to operate under ultraviolet lighting, avoids the risk of the operating condition of acid oxidase high temperature and pressure,
The controllability of operation is also improved.
(3), synthesis material is few, avoids the use of metal ion, and uses nano-film filtration technology, make resultant metal from
Son reaches 0.01ppm rank.
(4), synthesis step is few, and low energy consumption for short preparation period, simple process, overall process organic solvent-free, oxidant conversion
After only generate water, it is environmentally protective nontoxic, it is easy to industrialized production.
(5), using nanometer wet process powder technology, make material in stator and rotor in narrow gap by strong machinery and
The comprehensive function of liquid shear, centrifugation extruding, liquid layer friction, shock tearing and turbulent flow etc., so that 6-FXP is equal in water after crushing
It is more than even dispersion for 24 hours.Avoid the problem that nanometer powder is easy to reunite in the solution, dispersion is uneven.
(6), vacuum microwave dehydrating technology, have heating thermal inertia it is small, heating instantaneity, it is easily controllable, do not preheat
The advantages such as process.The heating for carrying out penetrability to material using microwave, improves the temperature of material, so that 6- within the shortest time
FTA rapid dehydration reacts to obtain 6-FDA.Solve the problems, such as long-time high temperature appearance color it is relatively deep and in melting it is blocky and
It is in crystalloid that chemical method, which is dehydrated dianhydride, and appearance color is shallower, the low problem of yield.
Detailed description of the invention
Fig. 1 is the HPLC spectrogram that 6-FTA is prepared in the embodiment of the present invention 1.
Fig. 2 is the HPLC spectrogram that 6-FDA is prepared in the embodiment of the present invention 1.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but not to limit the present invention.It should be pointed out that coming to those skilled in the art
It says, within spirit of that invention and thinking principle, various modifications and improvements can be made.These belong to protection of the invention
Range.
Embodiment 1:
A kind of preparation method of 4,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids comprising following steps:
It is first that the granular 4,4'- of 100g (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) are nano-milled in wet type
In dispersion machine with 20g water grinding dispersion；The power of nanometer wet process disintegrator is 12KW, fineness 80nm of crushing rear material or so.
Nanoscale 4,4'- (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) and 120g mass after taking 100g to disperse are dense
Degree is separately added into evenly dispersed in Photoreactor for 80% aqueous hydrogen peroxide solution, and then 10 DEG C, normal pressure opens the wave of 2Kw
The cold ultraviolet light of the LED of a length of 380nm, the UV light-induced light source irradiation reaction solution of uv power react 2h, are then heated to
Reaction solution nano-film filtration device is filtered after 55 DEG C of oxidation reaction 4.2h, the aperture of nano-film filtration device is 12nm, to be cooled
It is filtered after to room temperature and obtains 6-FTA, 6- FTA purity 99.95%.
6-FTA is put into drying and dewatering 3h in the microwave vacuum baking oven of 1Kw and obtains 6-FDA product.Product purity
99.937%, yield 98.1%.
The 6-FDA being prepared in embodiment 1 is subjected to ICP-MS and detects metal ion, specific testing result is shown in Table 1:
Embodiment 2:
A kind of preparation method of 4,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids comprising following steps:
It is first that the granular 4,4'- of 100g (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) are nano-milled in wet type
In dispersion machine with 200g water grinding dispersion.The power of nanometer wet process disintegrator is 12KW, fineness 80nm of crushing rear material or so.
Nanoscale 4,4'- (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) and 48g mass after taking 100g to disperse are dense
Degree is separately added into evenly dispersed in Photoreactor for 80% aqueous hydrogen peroxide solution, and then -6 DEG C, normal pressure opens the wave of 2Kw
The cold ultraviolet light of the LED of a length of 320nm, the UV light-induced light source irradiation reaction solution of uv power react 2.5h, then reheat
Reaction solution nano-film filtration device is filtered after to 50 DEG C of oxidation reaction 12h, suction filtration obtains 6-FTA, 6- after being cooled to room temperature
FTA purity 99.93%.
6-FTA is put into drying and dewatering 0.2h in the microwave vacuum baking oven of 20Kw and obtains 6-FDA product.Product purity
99.910%, yield 97.8%.
Embodiment 3:
A kind of preparation method of 4,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids comprising following steps:
It is first that the granular 4,4'- of 100g (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) are nano-milled in wet type
In dispersion machine with 200g water grinding dispersion.The power of nanometer wet process disintegrator is 15KW, fineness 80nm of crushing rear material or so.
Nanoscale 4,4'- (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) and 77g mass after taking 100g to disperse are dense
Degree is separately added into evenly dispersed in Photoreactor for 50% aqueous hydrogen peroxide solution, and then 32 DEG C, normal pressure opens the wave of 15Kw
The cold ultraviolet light of the LED of a length of 400nm, the UV light-induced light source irradiation reaction solution of uv power react 1.2h, then reheat
Reaction solution nano-film filtration device is filtered after to 60 DEG C of oxidation reaction 2.4h, suction filtration obtains 6-FTA, 6- after being cooled to room temperature
FTA purity 99.92%.
6-FTA is put into drying and dewatering 3h in the microwave vacuum baking oven of 1Kw and obtains 6-FDA product.Product purity
99.918%, yield 97.5%.
Embodiment 4:
It is first that the granular 4,4'- of 100g (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) are nano-milled in wet type
In dispersion machine with 100g water grinding dispersion.
Nanoscale 4,4'- (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) and 96g concentration after taking 100g to disperse
60% aqueous hydrogen peroxide solution is separately added into evenly dispersed in Photoreactor, and then 15 DEG C, normal pressure, the wavelength for opening 8Kw is
The cold ultraviolet light of the LED of 350nm, the UV light-induced light source irradiation reaction solution of uv power react 2.2h, are then heated to 56
Reaction solution nano-film filtration device is filtered after DEG C oxidation reaction 3.8h, is cooled to after room temperature to filter and obtains 6-FTA, 6-FTA
Purity 99.90%.
6-FTA is put into drying and dewatering 1h in the microwave vacuum baking oven of 12Kw and obtains 6-FDA product.Product purity
99.89%, yield 97.2%.
Comparative example 1:
A kind of preparation method of 4,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids comprising following steps:
It is first that the granular 4,4'- of 100g (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) are nano-milled in wet type
In dispersion machine with 80g water grinding dispersion.The power of nanometer wet process disintegrator is 12KW, fineness 80nm of crushing rear material or so.
Nanoscale 4,4'- (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) and 116g mass after taking 100g to disperse are dense
Degree is separately added into evenly dispersed in Photoreactor for 55% aqueous hydrogen peroxide solution, and then 10 DEG C, normal pressure opens the wave of 1Kw
The cold ultraviolet light of the LED of a length of 310nm, the UV light-induced light source irradiation reaction solution of uv power react 2.5h, then reheat
Reaction solution nano-film filtration device is filtered after to 55 DEG C of oxidation reaction 12h, suction filtration obtains 6-FTA, 6- after being cooled to room temperature
FTA purity 56.2%.
6-FTA is put into drying and dewatering 1h in the microwave vacuum baking oven of 12Kw and obtains 6-FDA product.Product purity
52.3%, yield 61.5%.
Comparative example 2:
A kind of preparation method of 4,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids, step are as follows:
It is first that the granular 4,4'- of 100g (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) are nano-milled in wet type
In dispersion machine with 80g water grinding dispersion.The power of nanometer wet process disintegrator is 15KW, fineness 80nm of crushing rear material or so.
Nanoscale 4,4'- (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) and 127g mass after taking 100g to disperse are dense
Degree is separately added into evenly dispersed in Photoreactor for 50% aqueous hydrogen peroxide solution, and then 10 DEG C, normal pressure opens the wave of 1Kw
The cold ultraviolet light of the LED of a length of 410nm, the UV light-induced light source irradiation reaction solution of uv power react 2.5h, then reheat
Reaction solution nano-film filtration device is filtered after to 55 DEG C of oxidation reaction 12h, suction filtration obtains 6-FTA, 6- after being cooled to room temperature
FTA purity 53.2%.
6-FTA is put into drying and dewatering 1h in the microwave vacuum baking oven of 12Kw and obtains 6-FDA product.Product purity
50.8%, yield 58.7%.
Comparative example 3:
A kind of preparation method of 4,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids, step are as follows:
The mistake for being 78% 4,4'- (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) and 146g mass concentration of 100g
Oxidation aqueous solution of hydrogen, which is separately added into Photoreactor, to be dispersed, and then under normal pressure and 10 DEG C of reaction temperature, the wavelength for opening 1kw is
The cold ultraviolet light of the LED of 380nm, the UV light-induced light source irradiation reaction solution of uv power react 2.5h, are then heated to 55
Reaction solution nano-film filtration device is filtered after DEG C oxidation reaction 12h, is cooled to after room temperature to filter and obtains 6-FTA, 6-FTA is pure
Degree 45.3%.
6-FTA is put into drying and dewatering 1h in the microwave vacuum baking oven of 5Kw and obtains 6-FDA product.Product purity 42.2%,
Yield 38.2%.
Comparative example 4:
A kind of preparation method of 4,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids, step are as follows:
It is first that the granular 4,4'- of 100g (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) are nano-milled in wet type
In dispersion machine with 150g water grinding dispersion.The power of nanometer wet process disintegrator is 15KW, fineness 80nm of crushing rear material or so.
Nanoscale 4,4'- (hexafluoro isopropenyl)-two ortho-xylenes (6-FXP) and 62g concentration after taking 100g to disperse
75% aqueous hydrogen peroxide solution is separately added into evenly dispersed in Photoreactor, and then 10 DEG C, normal pressure, the wavelength for opening 15Kw is
The cold ultraviolet light of the LED of 380nm, the UV light-induced light source irradiation reaction solution of uv power react 2h, are then heated to 56 DEG C
Reaction solution nano-film filtration device is filtered after oxidation reaction 4.2h, suction filtration obtains 6-FTA after being cooled to room temperature, and 6-FTA is pure
Degree 99.90%.
6-FTA is put into drying and dewatering 6h in the conventional vacuum baking oven of 12Kw and obtains 6-FDA product.Product purity
99.77%, yield 96.8%.But product agglomerates, and needs pulverizer to be crushed, and product colour is deeper.To subsequent use
It has an impact.
It is elaborated although the present invention has passed through specific embodiment, this profession ordinary skill
Personnel should be understood that made on this basis without departing from any form of claims and the variation of details,
Belong to invention which is intended to be protected.
Claims (8)
- The preparation method of one kind 4,4 ' -1. (hexafluoro isopropyl alkene) two anhydride phthalic acids, it is characterised in that the following steps are included:By granular 4,4'- (hexafluoro isopropenyl)-two ortho-xylenes in the nano-milled dispersion machine of wet type with broken point of pigment It dissipates；After dispersion nanoscale 4,4'- (hexafluoro isopropenyl)-two ortho-xylenes and aqueous hydrogen peroxide solution be separately added into light It is evenly dispersed in reactor, then under reaction temperature appropriate, open the cold ultraviolet light of LED, UV light-induced light source irradiation reaction Liquid reacts certain time, then reheats oxidation reaction and after the completion filters reaction solution, filters obtain 6-FTA after cooling；6-FTA is put into drying and dewatering in microwave vacuum baking oven and obtains 6-FDA product.
- 2. the preparation method of as described in claim 14,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids, it is characterised in that: the wet type The power of nanometer wet process disintegrator is 0.08 ~ 20KW, and smashing fineness is 10 ~ 100nm, 4,4'- (hexafluoro isopropenyl)-two neighbours two The weight ratio of toluene and water is 100::20 ~ 200.
- 3. the preparation method of as described in claim 14,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids, it is characterised in that: the peroxide The mass concentration for changing aqueous solution of hydrogen is 50% ~ 80%, 4,4'- (hexafluoro isopropenyl)-two ortho-xylene dispersion liquids and hydrogen peroxide The mass ratio of aqueous solution is 100:48 ~ 192.
- 4. the preparation method of as described in claim 14,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids, it is characterised in that: institute in step b The reaction temperature stated is -6 ~ 32 DEG C, and reaction pressure is normal pressure, after reacting 1.2 ~ 2.5h, is heated to 50 ~ 60 DEG C, the reaction was continued 2.4~12h。
- 5. the preparation method of as described in claim 14,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids, it is characterised in that: the cold purple Outer light is long wave ultraviolet light lamp, and wavelength 320-400nm, power is 0.1 ~ 20KW.
- 6. the preparation method of as described in claim 14,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids, it is characterised in that: the filtering Device is nano-film filtration device, aperture 12nm.
- 7. the preparation method of as described in claim 14,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids, it is characterised in that: the microwave The microwave frequency of vacuum drying oven is 2.45GHz ± 25MHz, and dewatering time is 0.2 ~ 3h.
- 8. the preparation method of as described in claim 14,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acids, it is characterised in that: be prepared 4,4 '-(hexafluoro isopropyl alkene) two anhydride phthalic acid yields reach 98.1%, purity 99.937%, metal ion reaches 0.01ppm grades Not.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111333601A (en) * | 2020-05-21 | 2020-06-26 | 山东冠森高分子材料科技股份有限公司 | Method for preparing 4, 4' - (hexafluoroisopropenyl) diphthalic anhydride |
| CN113004140A (en) * | 2021-03-18 | 2021-06-22 | 天津市泰合利华材料科技有限公司 | Method for synthesizing 4,4' - (perfluoropropane-2, 2-diyl) diphthalic acid |
| CN114315568A (en) * | 2021-12-30 | 2022-04-12 | 山东华夏神舟新材料有限公司 | 4,4' - (hexafluoroisopropylene) diphthalic acid and preparation method thereof |
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| CN107698436A (en) * | 2016-08-09 | 2018-02-16 | 朱翠英 | A kind of method for preparing the more formic acid analog derivatives of aromatic hydrocarbons |
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| CN113004140B (en) * | 2021-03-18 | 2022-09-30 | 天津众泰材料科技有限公司 | Method for synthesizing 4,4' - (perfluoropropane-2, 2-diyl) diphthalic acid |
| CN114315568A (en) * | 2021-12-30 | 2022-04-12 | 山东华夏神舟新材料有限公司 | 4,4' - (hexafluoroisopropylene) diphthalic acid and preparation method thereof |
| CN114315568B (en) * | 2021-12-30 | 2024-01-12 | 山东华夏神舟新材料有限公司 | 4,4' -hexafluoro-isopropenyl-isophthalic acid and preparation method thereof |
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