CN110408002A - Preparation method based on automotive hub film epoxy resin - Google Patents
Preparation method based on automotive hub film epoxy resin Download PDFInfo
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- CN110408002A CN110408002A CN201910798142.XA CN201910798142A CN110408002A CN 110408002 A CN110408002 A CN 110408002A CN 201910798142 A CN201910798142 A CN 201910798142A CN 110408002 A CN110408002 A CN 110408002A
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- epoxy resin
- preparation
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- reaction kettle
- automotive hub
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/02—Polycondensates containing more than one epoxy group per molecule
- C08G59/022—Polycondensates containing more than one epoxy group per molecule characterised by the preparation process or apparatus used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/02—Polycondensates containing more than one epoxy group per molecule
- C08G59/04—Polycondensates containing more than one epoxy group per molecule of polyhydroxy compounds with epihalohydrins or precursors thereof
- C08G59/06—Polycondensates containing more than one epoxy group per molecule of polyhydroxy compounds with epihalohydrins or precursors thereof of polyhydric phenols
- C08G59/063—Polycondensates containing more than one epoxy group per molecule of polyhydroxy compounds with epihalohydrins or precursors thereof of polyhydric phenols with epihalohydrins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/91—Polymers modified by chemical after-treatment
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Epoxy Resins (AREA)
Abstract
The present invention provides the preparation method based on automotive hub film epoxy resin, distilled water and bisphenol-A is added in reaction kettle according to the proportion, turn on agitator, then propylene oxide, polyester and liquid alkaline is added to be added in reaction kettle according to the proportion respectively, under conditions of 95 degree, reacts 2 hours, macromolecule epoxy resin is prepared, then distilled water is added to be washed, it washes repeatedly, is dehydrated, is cooled down, solid epoxy resin is prepared, then it is sliced, finished product is prepared.The present invention is by being added hydroxy-terminated polyester, with excessive epoxychloropropane, contain hydroxy-terminated polyester in the macromolecule epoxy resin prepared, to reduce epoxy resin preparation cost, and increase toughness, and by reducing reaction temperature, guarantees that excess epoxy chloropropane does not react, reduce the heat release situation of initial reaction stage, slow down reaction speed, ring-opening reaction degree is reduced, reduces epoxy resin cost, and increase toughness.
Description
Technical field
The present invention relates to chemical technology fields, more particularly to the preparation method based on automotive hub film epoxy resin.
Background technique
Epoxy resin is the organic high molecular compound referred in molecule containing two or more epoxy groups, it can
It is crosslinked with a plurality of types of curing agent and reacts to form insoluble, insoluble three-dimensional net structure polymer, with excellent
Mechanical property, adhesive property, electrical insulation properties and chemical resistance, therefore in coating, food, chemical industry, anti-corrosion, machine
What the fields such as tool, electronics, electrical all obtained is widely applied.
However, the selection of hub surface film is particularly important when epoxy resin is used into automotive hub, hub surface is applied
Film is in addition to having required good surface quality and application property, it is also necessary to excellent mechanical performance, good bottom horizontal flow sheet, i.e., by force
Tough degree, and existing epoxy resin does not have the function of can be used on wheel hub also.
Therefore, invention is necessary to solve the above problems based on the preparation method of automotive hub film epoxy resin
Summary of the invention
The purpose of the present invention is to provide the preparation methods based on automotive hub film epoxy resin, to solve above-mentioned skill
Art problem.
The present invention using following technical scheme in order to solve the above technical problems, realized:
Based on the preparation method of automotive hub film epoxy resin, the weight part ratio of the preparation formula of the epoxy resin
Are as follows: 1000 parts of bisphenol-A, 677 parts of liquid alkaline, 510-540 parts of epoxychloropropane, 51-54 parts of polyester and 1500 parts of distilled water, the liquid
Sodium hydrate aqueous solution, 40% hydrochloride aqueous solution and the distilled water that alkali is 32% configure, epoxy resin preparation method
Are as follows: distilled water and bisphenol-A are added in reaction kettle, turn on agitator according to the proportion, propylene oxide, polyester and liquid alkaline is then added
It is added in reaction kettle according to the proportion respectively, under conditions of 95 degree, reacts 2 hours, macromolecule epoxy resin is prepared, then
Distilled water is added to be washed, washes repeatedly, is dehydrated, is cooled down, solid epoxy resin is prepared, is then sliced,
Finished product is prepared.
Preferably, the polyester is hydroxy-terminated polyester setting, and the epoxychloropropane is excessive setting, makes epoxy resin
It can be mixed with a part of hydroxy-terminated polyester after discharging, reduce cost, and increase toughness.
Preferably, the distilled water and bisphenol-A are heated to being added under conditions of 43-45 degree inside reaction kettle, work as reaction
Kettle temperature degree, which is reheated to, propylene oxide and polyester to be added under conditions of 43-45 degree.
Preferably, the mode that the sodium hydrate aqueous solution in the liquid alkaline is slowly added dropwise is added into reaction kettle, is reacting
Kettle internal temperature rises to 95 and is added dropwise.
Preferably, the sodium-chloride water solution in the liquid alkaline is within a hour after sodium hydrate aqueous solution is added dropwise
Portion is added dropwise, and what wherein this belonged in 2 in epoxy resin preparation process hours for 1 hour is arranged for 1 hour.
Preferably, the mass ratio between the epoxychloropropane and polyester is 10:1.
Preferably, the washing times of the epoxy resin are 6 times, and open the blender in reaction kettle before washing, often
Washing time is 25-28 minutes.
Preferably, the epoxy resin dehydration is vacuum dehydration, and vacuum degree is -0.078MPa, and dewatering time is 50-
55 minutes.
Preferably, the discharging speed of the epoxy resin in a kettle is 30kg/min, reacts discharging speed by increasing
Degree, the further reaction of condition of high temperature when avoiding discharging.
The beneficial effects of the present invention are:
(1) present invention is conducive to the high score for making to prepare by the way that hydroxy-terminated polyester and excessive epoxychloropropane is added
Contain hydroxy-terminated polyester in sub- epoxy resin, to reduce epoxy resin preparation cost, and increase toughness, and passing through will be anti-
It answers temperature to reduce, guarantees that excess epoxy chloropropane does not react, reduce the heat release situation of initial reaction stage, slow down reaction speed, reduce
Ring-opening reaction degree reduces epoxy resin cost, and increases toughness.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained, and however, the following embodiments are merely preferred embodiments of the present invention, and not all.
Based on the implementation example in the implementation mode, those skilled in the art's obtained other realities without making creative work
Example is applied, protection scope of the present invention is belonged to.Experimental method in following embodiments is unless otherwise specified conventional method,
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment one:
The present invention provides the preparation method based on automotive hub film epoxy resin, the preparation of the epoxy resin is matched
The weight part ratio of side are as follows: 1000 parts of bisphenol-A, 677 parts of liquid alkaline, 510 parts of epoxychloropropane, 51 parts of polyester and 1500 parts of distilled water,
Sodium hydrate aqueous solution, 40% hydrochloride aqueous solution and the distilled water that the liquid alkaline is 32% configure, and the polyester is hydroxyl
The setting of base end capped polyesters, the epoxychloropropane are excessive setting, and epoxy resin inside reaction kettle the preparation method comprises the following steps: by heating
When being spent to 43-45, distilled water and bisphenol-A are added in reaction kettle according to the proportion, turn on agitator, when temperature of reaction kettle adds again
Heat is added in reaction kettle according to the proportion respectively to propylene oxide and polyester by 43-45 degree, is then added, and by the hydrogen in liquid alkaline
Aqueous solution of sodium oxide is slowly added dropwise into reaction kettle, rises to 95 in reaction kettle internal temperature and is added dropwise, in 95 degree of condition
Under, sodium-chloride water solution is added dropwise inside a hour after sodium hydrate aqueous solution is added dropwise, is reacted 2 hours,
Macromolecule epoxy resin is prepared, distilled water is then added and is washed, washes 6 times repeatedly, carries out vacuum dehydration, cooling,
Solid epoxy resin is prepared, is then sliced, finished product is prepared.
Embodiment two:
Based on the preparation method of automotive hub film epoxy resin, the weight part ratio of the preparation formula of the epoxy resin
Are as follows: 1000 parts of bisphenol-A, 677 parts of liquid alkaline, 520 parts of epoxychloropropane, 52 parts of polyester and 1500 parts of distilled water, the liquid alkaline are
32% sodium hydrate aqueous solution, 40% hydrochloride aqueous solution and distilled water configure, and the polyester is hydroxy-terminated polyester
Setting, the epoxychloropropane are excessive setting, and epoxy resin is the preparation method comprises the following steps: 43-45 degree will be heated to inside reaction kettle
When, distilled water and bisphenol-A are added in reaction kettle according to the proportion, turn on agitator, when temperature of reaction kettle is reheated to 43-
45 degree, propylene oxide and polyester is then added and is added in reaction kettle according to the proportion respectively, and by the sodium hydroxide water in liquid alkaline
Solution is slowly added dropwise into reaction kettle, rises to 95 in reaction kettle internal temperature and is added dropwise, under conditions of 95 degree, by chlorination
Sodium water solution is added dropwise inside a hour after sodium hydrate aqueous solution is added dropwise, and reacts 2 hours, height is prepared
Then molecule epoxy resin is added distilled water and is washed, wash 6 times repeatedly, carry out vacuum dehydration, cooling, is prepared solid
State epoxy resin, is then sliced, and finished product is prepared.
Embodiment three:
Based on the preparation method of automotive hub film epoxy resin, the weight part ratio of the preparation formula of the epoxy resin
Are as follows: 1000 parts of bisphenol-A, 677 parts of liquid alkaline, 530 parts of epoxychloropropane, 53 parts of polyester and 1500 parts of distilled water, the liquid alkaline are
32% sodium hydrate aqueous solution, 40% hydrochloride aqueous solution and distilled water configure, and the polyester is hydroxy-terminated polyester
Setting, the epoxychloropropane are excessive setting, and epoxy resin is the preparation method comprises the following steps: 43-45 degree will be heated to inside reaction kettle
When, distilled water and bisphenol-A are added in reaction kettle according to the proportion, turn on agitator, when temperature of reaction kettle is reheated to 43-
45 degree, propylene oxide and polyester is then added and is added in reaction kettle according to the proportion respectively, and by the sodium hydroxide water in liquid alkaline
Solution is slowly added dropwise into reaction kettle, rises to 95 in reaction kettle internal temperature and is added dropwise, under conditions of 95 degree, by chlorination
Sodium water solution is added dropwise inside a hour after sodium hydrate aqueous solution is added dropwise, and reacts 2 hours, height is prepared
Then molecule epoxy resin is added distilled water and is washed, wash 6 times repeatedly, carry out vacuum dehydration, cooling, is prepared solid
State epoxy resin, is then sliced, and finished product is prepared.
Example IV:
Based on the preparation method of automotive hub film epoxy resin, the weight part ratio of the preparation formula of the epoxy resin
Are as follows: 1000 parts of bisphenol-A, 677 parts of liquid alkaline, 540 parts of epoxychloropropane, 54 parts of polyester and 1500 parts of distilled water, the liquid alkaline are
32% sodium hydrate aqueous solution, 40% hydrochloride aqueous solution and distilled water configure, and the polyester is hydroxy-terminated polyester
Setting, the epoxychloropropane are excessive setting, and epoxy resin is the preparation method comprises the following steps: 43-45 degree will be heated to inside reaction kettle
When, distilled water and bisphenol-A are added in reaction kettle according to the proportion, turn on agitator, when temperature of reaction kettle is reheated to 43-
45 degree, propylene oxide and polyester is then added and is added in reaction kettle according to the proportion respectively, and by the sodium hydroxide water in liquid alkaline
Solution is slowly added dropwise into reaction kettle, rises to 95 in reaction kettle internal temperature and is added dropwise, under conditions of 95 degree, by chlorination
Sodium water solution is added dropwise inside a hour after sodium hydrate aqueous solution is added dropwise, and reacts 2 hours, height is prepared
Then molecule epoxy resin is added distilled water and is washed, wash 6 times repeatedly, carry out vacuum dehydration, cooling, is prepared solid
State epoxy resin, is then sliced, and finished product is prepared.
Physical and chemical performance detection is carried out to the epoxy resin product that embodiment 1-4 is prepared, result is as shown in table 1 below,
As it can be seen from table 1 using addition hydroxy-terminated polyester, and excessive epoxychloropropane is added, advantageously reduce epoxy resin
Cost, and increase toughness, and in order to guarantee that excess epoxy chloropropane does not react, therefore reaction temperature is compared into common asphalt mixtures modified by epoxy resin
Rouge reduces, and reduces the heat release situation of initial reaction stage, slows down reaction speed, reduces ring-opening reaction degree, reduces epoxy resin cost,
And increase toughness.
The performance test results of 1 epoxy resin of table:
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
For personnel it should be appreciated that the present invention is not limited to the above embodiments, described in the above embodiment and specification is only the present invention
Preference, be not intended to limit the invention, without departing from the spirit and scope of the present invention, the present invention also has various
Changes and improvements, these changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by institute
Attached claims and its equivalent thereof.
Claims (9)
1. the preparation method based on automotive hub film epoxy resin, it is characterised in that: the preparation formula of the epoxy resin
Weight part ratio are as follows: 1000 parts of bisphenol-A, 677 parts of liquid alkaline, 510-540 parts of epoxychloropropane, 51-54 parts of polyester and distilled water
1500 parts, sodium hydrate aqueous solution, 40% hydrochloride aqueous solution and the distilled water that the liquid alkaline is 32% configure, epoxy
Process for preparing resins are as follows: distilled water and bisphenol-A are added in reaction kettle, turn on agitator according to the proportion, epoxy third is then added
Alkane, polyester and liquid alkaline are added in reaction kettle according to the proportion respectively, under conditions of 95 degree, react 2 hours, macromolecule is prepared
Then epoxy resin is added distilled water and is washed, washes repeatedly, be dehydrated, cooled down, solid epoxy resin is prepared,
Then it is sliced, finished product is prepared.
2. the preparation method according to claim 1 based on automotive hub film epoxy resin, it is characterised in that: described
Polyester is hydroxy-terminated polyester setting, and the epoxychloropropane is excessive setting.
3. the preparation method according to claim 1 based on automotive hub film epoxy resin, it is characterised in that: described
Distilled water and bisphenol-A are heated to being added under conditions of 43-45 degree inside reaction kettle, when temperature of reaction kettle be reheated to by
Propylene oxide and polyester are added under conditions of 43-45 degree.
4. the preparation method according to claim 1 based on automotive hub film epoxy resin, it is characterised in that: described
The mode that sodium hydrate aqueous solution in liquid alkaline is slowly added dropwise is added into reaction kettle, rises to 95 drops in reaction kettle internal temperature
It adds complete.
5. the preparation method according to claim 1 based on automotive hub film epoxy resin, it is characterised in that: described
Sodium-chloride water solution in liquid alkaline is added dropwise inside a hour after sodium hydrate aqueous solution is added dropwise, wherein this 1
What hour belonged in 2 in epoxy resin preparation process hours is arranged for 1 hour.
6. the preparation method according to claim 1 based on automotive hub film epoxy resin, it is characterised in that: described
Mass ratio between epoxychloropropane and polyester is 10:1.
7. the preparation method according to claim 1 based on automotive hub film epoxy resin, it is characterised in that: described
The washing times of epoxy resin are 6 times, and open the blender in reaction kettle before washing, and washing time is 25-28 each time
Minute.
8. the preparation method according to claim 1 based on automotive hub film epoxy resin, it is characterised in that: described
Epoxy resin dehydration is vacuum dehydration, and vacuum degree is -0.078MPa, and dewatering time is 50-55 minutes.
9. the preparation method according to claim 1 based on automotive hub film epoxy resin, it is characterised in that: described
The discharging speed of epoxy resin in a kettle is 30kg/min.
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CN201910798142.XA CN110408002A (en) | 2019-08-27 | 2019-08-27 | Preparation method based on automotive hub film epoxy resin |
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CN201910798142.XA CN110408002A (en) | 2019-08-27 | 2019-08-27 | Preparation method based on automotive hub film epoxy resin |
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1675330A (en) * | 2002-08-19 | 2005-09-28 | 3M创新有限公司 | Epoxy compositions having improved shelf life and articles containing the same |
WO2009140001A1 (en) * | 2008-05-14 | 2009-11-19 | Dow Global Technologies Inc. | Epoxy toughening using linear co-polyesters |
CN104448267A (en) * | 2014-12-23 | 2015-03-25 | 南京林业大学 | Method for preparing solid epoxy resin toughened polyester |
CN104448236A (en) * | 2014-12-29 | 2015-03-25 | 南京林业大学 | Preparation method of epoxy resin |
-
2019
- 2019-08-27 CN CN201910798142.XA patent/CN110408002A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1675330A (en) * | 2002-08-19 | 2005-09-28 | 3M创新有限公司 | Epoxy compositions having improved shelf life and articles containing the same |
WO2009140001A1 (en) * | 2008-05-14 | 2009-11-19 | Dow Global Technologies Inc. | Epoxy toughening using linear co-polyesters |
CN104448267A (en) * | 2014-12-23 | 2015-03-25 | 南京林业大学 | Method for preparing solid epoxy resin toughened polyester |
CN104448236A (en) * | 2014-12-29 | 2015-03-25 | 南京林业大学 | Preparation method of epoxy resin |
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