CN108299935A - A kind of preparation method of the filler of reinforced resin coating intensity - Google Patents
A kind of preparation method of the filler of reinforced resin coating intensity Download PDFInfo
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- CN108299935A CN108299935A CN201810094589.4A CN201810094589A CN108299935A CN 108299935 A CN108299935 A CN 108299935A CN 201810094589 A CN201810094589 A CN 201810094589A CN 108299935 A CN108299935 A CN 108299935A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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Abstract
The invention discloses a kind of preparation methods of the filler of reinforced resin coating intensity, include the following steps：（1）Filler cleaning treatment,（2）Calcination processing,（3）Modified solution preparation,（4）Modification.The present invention has carried out special modified optimization to bentonite and has handled, significantly improve bentonitic surface-active and the compatible binding ability between resin matrix, reduce the problems such as bentonite clay particle filler is easily reunited, dispersion effect is bad, effectively improve the performances such as the mechanical strength of cold coating, great application value.
Description
Technical field
The invention belongs to high-molecular coating technical fields, and in particular to a kind of preparation of the filler of reinforced resin coating intensity
Method.
Background technology
Use of the coating in modern people live is extensive, can not only improve the appearance condition of part product, while can also
It promotes it and uses quality.Epoxy resin has the performances such as excellent bonding, corrosion-resistant, insulation, is widely used in coating.Due to
Epoxy resin composite material has the characteristics that intensity is higher, low density, has been increasingly becoming the indispensable basis of industrial circle
One of material.However epoxide resin material makes it answer in heat resistance, wearability, dimensional stability, brittleness etc. Shortcomings
With being affected.In order to improve the quality of coating, people add into coating and have used inorganic filler components, to improve coating
Whole physicochemical property, because inorganic filler particle is small, easy reunion, leads to dispersion effect not although achieving certain effect
Good, the corresponding improvement for qualities such as the mechanics of coating is still had large improvement space, to this people when its filling uses
Surface modification treatment can be carried out, most common is exactly to carry out surface coupling modifier processing with silane coupling agent, although improving nothing
The filling of machine filler uses quality, but with the continuous promotion that people require coating property, conventional surface modification treatment
Method can no longer meet the demand that design uses.
Invention content
The purpose of the present invention is for existing problem, provide a kind of preparation side of the filler of reinforced resin coating intensity
Method.
The present invention is achieved by the following technical solutions：
A kind of preparation method of the filler of reinforced resin coating intensity, includes the following steps：
（1）Filler cleaning treatment：
Bentonite is first immersed in 8 ~ 10min of processing in salpeter solution, filters out rinsed one time with clear water after the completion, then place into
It is spare that 35 ~ 40min is dried in drying box；
（2）Calcination processing：
By step（1）Treated, and bentonite is put into progress calcination processing in calcining furnace, during which controls the temperature in calcining furnace
It is 800 ~ 860 DEG C, is taken out after 1 ~ 1.5h spare；
（3）It is prepared by modified solution：
A. methyl linoleate and glycerine are put into reaction kettle jointly, be then added its gross mass 1 ~ 3% potassium hydroxide, 1.5
~ 2.5% magnesium hydroxide after being stirred continuously 10 ~ 15min of processing, then alkyl phenol polyoxyethylene ether is added into reaction kettle, simultaneously
The temperature heating of reaction kettle is remained 73 ~ 78 DEG C, and the pressure in reaction kettle is risen into 0.2 ~ 0.3MPa, is stirred continuously processing
Taken out after 40 ~ 45min modification liquid A is spare；
B. by cetyl trimethylammonium bromide and dodecyl sodium sulfate according to weight ratio 2:1 is put into agitator tank jointly,
It is 33 ~ 37 DEG C that heating, which is kept stirring temperature in tank, be stirred continuously after 25 ~ 30min of mixed processing take out modification liquid B is spare；
（4）Modification：
A. by step（2）Treated, and bentonite puts into step（3）It operates in modification liquid A made from a, heating keeps modification liquid
The temperature of A is 55 ~ 60 DEG C, is filtered out after being stirred continuously 40 ~ 45min of processing, is then placed in the environment that temperature is 70 ~ 75 DEG C and does
15 ~ 20min of dry processing, takes out spare after the completion；
B. will operation a treated that bentonite puts into step（3）It operates in modification liquid B made from b, heating keeps modification liquid B
Temperature be 75 ~ 80 DEG C, filtered out after being stirred continuously 20 ~ 25min of processing, it is to be done in 85 ~ 90 DEG C of environment to be then placed in temperature
55 ~ 60min of dry processing takes out after the completion.
Further, step（1）Described in salpeter solution in nitric acid mass fraction be 3 ~ 5%.
Further, step（1）Described in drying process when control drying box in temperature be 100 ~ 110 DEG C.
Further, step（3）It is 2.4 ~ 2.6 to operate the molar ratio that methyl linoleate and glycerine described in a are blended:1.
Further, step（3）The addition for operating the alkyl phenol polyoxyethylene ether described in a is the total matter of methyl linoleate
The 32 ~ 35% of amount.
Further, step（3）It is 800 ~ 900 revs/min to operate the speed of agitator for being stirred processing described in b.
Further, step（4）The speed of agitator for operating the stir process described in a is 1500 ~ 1800 revs/min.
Further, step（4）The speed of agitator for operating the stir process described in b is 2200 ~ 2500 revs/min.
Then the present invention has carried out it special modification using bentonite as the matrix composition of filler, wherein first matching
It is with methyl linoleate, glycerine, alkyl phenol polyoxy to have made two kinds of characteristics different modification liquid A and modification liquid B, wherein modification liquid A
A kind of linoleic acid ester APEO activator solution obtained is blended in vinethene, uses it as matrix dressing agent to swelling
Soil has carried out a modification, has reconciled the amphipathic property on bentonite surface, and intercalation is that subsequent modification is established in interlayer
Basis is determined, modification liquid B is compounded with cationic cetyl trimethylammonium bromide and anionic dodecyl sodium sulfate
It is made, uses it as dressing agent is improved and twice-modified processing has been carried out to bentonite, further improve the anti-of bentonite surface
Activity, and the compatibility between resin matrix are answered, while also improving bentonitic absorption crystallized ability, it is solid in cold coating
The binding ability and mechanical characteristic of net high-polymer interchain are enhanced when change.
The present invention has the following advantages compared with prior art：
The present invention has carried out special modified optimization to bentonite and has handled, hence it is evident that improve bentonitic surface-active and with tree
Compatible binding ability between aliphatic radical body, reduces the problems such as bentonite clay particle filler is easily reunited, dispersion effect is bad, is effectively improved
The performances such as the mechanical strength of cold coating, great application value.
Specific implementation mode
Embodiment 1
A kind of preparation method of the filler of reinforced resin coating intensity, includes the following steps：
（1）Filler cleaning treatment：
First bentonite is immersed in salpeter solution and handles 8min, filters out rinsed one time with clear water after the completion, then place into
It is spare that 35min is dried in drying box；
（2）Calcination processing：
By step（1）Treated, and bentonite is put into progress calcination processing in calcining furnace, during which controls the temperature in calcining furnace
It is 800 DEG C, is taken out after 1h spare；
（3）It is prepared by modified solution：
A. methyl linoleate and glycerine are put into reaction kettle jointly, be then added its gross mass 1% potassium hydroxide, 1.5%
Magnesium hydroxide then alkyl phenol polyoxyethylene ether is added into reaction kettle after being stirred continuously processing 10min, while by reaction kettle
Temperature heating remain 73 DEG C, and the pressure in reaction kettle is risen into 0.2MPa, takes out to change after being stirred continuously processing 40min
Property liquid A is spare；
B. by cetyl trimethylammonium bromide and dodecyl sodium sulfate according to weight ratio 2:1 is put into agitator tank jointly,
It is 33 DEG C that heating, which is kept stirring temperature in tank, be stirred continuously after mixed processing 25min take out modification liquid B is spare；
（4）Modification：
A. by step（2）Treated, and bentonite puts into step（3）It operates in modification liquid A made from a, heating keeps modification liquid
The temperature of A is 55 DEG C, is filtered out after being stirred continuously processing 40min, is then placed in the environment that temperature is 70 DEG C and is dried
15min takes out spare after the completion；
B. will operation a treated that bentonite puts into step（3）It operates in modification liquid B made from b, heating keeps modification liquid B
Temperature be 75 DEG C, filtered out after being stirred continuously processing 20min, it is to be dried in 85 DEG C of environment to be then placed in temperature
55min takes out after the completion.
Further, step（1）Described in salpeter solution in nitric acid mass fraction be 3%.
Further, step（1）Described in drying process when control drying box in temperature be 100 DEG C.
Further, step（3）It is 2.4 to operate the molar ratio that methyl linoleate and glycerine described in a are blended:1.
Further, step（3）The addition for operating the alkyl phenol polyoxyethylene ether described in a is the total matter of methyl linoleate
The 32% of amount.
Further, step（3）It is 800 revs/min to operate the speed of agitator for being stirred processing described in b.
Further, step（4）The speed of agitator for operating the stir process described in a is 1500 revs/min.
Further, step（4）The speed of agitator for operating the stir process described in b is 2200 revs/min.
Embodiment 2
A kind of preparation method of the filler of reinforced resin coating intensity, includes the following steps：
（1）Filler cleaning treatment：
First bentonite is immersed in salpeter solution and handles 9min, filters out rinsed one time with clear water after the completion, then place into
It is spare that 37min is dried in drying box；
（2）Calcination processing：
By step（1）Treated, and bentonite is put into progress calcination processing in calcining furnace, during which controls the temperature in calcining furnace
It is 830 DEG C, is taken out after 1.2h spare；
（3）It is prepared by modified solution：
A. methyl linoleate and glycerine are put into reaction kettle jointly, be then added its gross mass 2% potassium hydroxide, 2%
Magnesium hydroxide then alkyl phenol polyoxyethylene ether is added into reaction kettle after being stirred continuously processing 13min, while by reaction kettle
Temperature heating remains 77 DEG C, and the pressure in reaction kettle is risen to 0.25MPa, takes out to change after being stirred continuously processing 43min
Property liquid A is spare；
B. by cetyl trimethylammonium bromide and dodecyl sodium sulfate according to weight ratio 2:1 is put into agitator tank jointly,
It is 36 DEG C that heating, which is kept stirring temperature in tank, be stirred continuously after mixed processing 28min take out modification liquid B is spare；
（4）Modification：
A. by step（2）Treated, and bentonite puts into step（3）It operates in modification liquid A made from a, heating keeps modification liquid
The temperature of A is 58 DEG C, is filtered out after being stirred continuously processing 43min, is then placed in the environment that temperature is 72 DEG C and is dried
17min takes out spare after the completion；
B. will operation a treated that bentonite puts into step（3）It operates in modification liquid B made from b, heating keeps modification liquid B
Temperature be 78 DEG C, filtered out after being stirred continuously processing 22min, it is to be dried in 87 DEG C of environment to be then placed in temperature
58min takes out after the completion.
Further, step（1）Described in salpeter solution in nitric acid mass fraction be 4%.
Further, step（1）Described in drying process when control drying box in temperature be 105 DEG C.
Further, step（3）It is 2.5 to operate the molar ratio that methyl linoleate and glycerine described in a are blended:1.
Further, step（3）The addition for operating the alkyl phenol polyoxyethylene ether described in a is the total matter of methyl linoleate
The 34% of amount.
Further, step（3）It is 860 revs/min to operate the speed of agitator for being stirred processing described in b.
Further, step（4）The speed of agitator for operating the stir process described in a is 1700 revs/min.
Further, step（4）The speed of agitator for operating the stir process described in b is 2400 revs/min.
Embodiment 3
A kind of preparation method of the filler of reinforced resin coating intensity, includes the following steps：
（1）Filler cleaning treatment：
First bentonite is immersed in salpeter solution and handles 10min, filters out rinsed one time with clear water after the completion, then place into
It is spare that 40min is dried in drying box；
（2）Calcination processing：
By step（1）Treated, and bentonite is put into progress calcination processing in calcining furnace, during which controls the temperature in calcining furnace
It is 860 DEG C, is taken out after 1.5h spare；
（3）It is prepared by modified solution：
A. methyl linoleate and glycerine are put into reaction kettle jointly, be then added its gross mass 3% potassium hydroxide, 2.5%
Magnesium hydroxide then alkyl phenol polyoxyethylene ether is added into reaction kettle after being stirred continuously processing 15min, while by reaction kettle
Temperature heating remain 78 DEG C, and the pressure in reaction kettle is risen into 0.3MPa, takes out to change after being stirred continuously processing 45min
Property liquid A is spare；
B. by cetyl trimethylammonium bromide and dodecyl sodium sulfate according to weight ratio 2:1 is put into agitator tank jointly,
It is 37 DEG C that heating, which is kept stirring temperature in tank, be stirred continuously after mixed processing 30min take out modification liquid B is spare；
（4）Modification：
A. by step（2）Treated, and bentonite puts into step（3）It operates in modification liquid A made from a, heating keeps modification liquid
The temperature of A is 60 DEG C, is filtered out after being stirred continuously processing 45min, is then placed in the environment that temperature is 75 DEG C and is dried
20min takes out spare after the completion；
B. will operation a treated that bentonite puts into step（3）It operates in modification liquid B made from b, heating keeps modification liquid B
Temperature be 80 DEG C, be stirred continuously processing 25min after filter out, be then placed in environment at a temperature of 90 °C and be dried
60min takes out after the completion.
Further, step（1）Described in salpeter solution in nitric acid mass fraction be 5%.
Further, step（1）Described in drying process when control drying box in temperature be 110 DEG C.
Further, step（3）It is 2.6 to operate the molar ratio that methyl linoleate and glycerine described in a are blended:1.
Further, step（3）The addition for operating the alkyl phenol polyoxyethylene ether described in a is the total matter of methyl linoleate
The 35% of amount.
Further, step（3）It is 900 revs/min to operate the speed of agitator for being stirred processing described in b.
Further, step（4）The speed of agitator for operating the stir process described in a is 1800 revs/min.
Further, step（4）The speed of agitator for operating the stir process described in b is 2500 revs/min.
Comparative example 1
This comparative example 1 compared with Example 2, eliminates step（3）Modified solution preparation manipulation a and step（4）It is modified
The corresponding processing operations of processing operation a, method and step all same in addition to this.
Comparative example 2
This comparative example 2 compared with Example 2, eliminates step（3）Modified solution preparation manipulation b and step（4）It is modified
The corresponding processing operations of processing operation b, method and step all same in addition to this.
Comparative example 3
This comparative example 3 compared with Example 2, by step（4）Operation a and operation b process sequences in modification are carried out
It is reverse, method and step all same in addition to this.
Control group
Existing bentonite surface modifying treatment specifically first carries out calcination processing, then by ethyl alcohol, silane to bentonite
Coupling agent kh550, water are according to weight ratio 1:3:15 carry out being mixed to prepare treatment fluid, and the bentonite after calcining is immersed in treatment fluid
In, it is filtered out after ultrasonic disperse processing 30min, drying.
In order to compare effect of the present invention, selects with a collection of bentonite as experimental raw, then use above-described embodiment respectively
2, comparative example 1, comparative example 2, comparative example 3, the corresponding method of control group are modified processing, carry out after the completion
Performance test, specific correction data are as shown in table 1 below：
Table 1
| Specific surface area（m2g-1） | |
| Embodiment 2 | 12.1 |
| Comparative example 1 | 9.8 |
| Comparative example 2 | 10.2 |
| Comparative example 3 | 10.7 |
| Control group | 8.9 |
Treated that bentonitic characterization of adsorption has fine enhancing, surface-active etc. to be corresponding with by the present invention it can be seen from upper table 1
Improve well.Bentonite eliminated in structural analysis discovery comparative example 1 and changes after to above-mentioned each group process
The processing of property liquid A, loses attachment, the complex matrix of successive modified processing, reduces treatment effect；And comparative example 2 is then
Follow-up compound modification again is not carried out, and effect promoting is also limited, and comparative example 3 is because modification liquid B component occupies absorption
Site, causes modification liquid A, the ingredient of modification liquid B fails effective compound fixation, equally causes declining to a great extent for performance.
It is in order to further compare effect of the present invention, above-described embodiment 2, comparative example 1, comparative example 2, comparison is real
It applies the modified alta-mud after example 3, control group alignment processing to be used in the making of coating, specifically by epoxy resin, bentone
Soil, curing agent, thixotropic agent are corresponded to according to weight ratio 100:18:3:2, which carry out mixing, is put into agitator tank, with 1300 revs/min
Rotating speed stir process 1.5h after take out, be made coating, finally the characteristic of coating is tested, specific correction data such as following table
Shown in 2：
Table 2
| Hardness after solidification（H） | Wearability（Ten thousand times） | |
| Embodiment 2 | 8H | 7.3 |
| Comparative example 1 | 5H | 6.0 |
| Comparative example 2 | 6H | 6.4 |
| Comparative example 3 | 6H | 6.7 |
| Control group | 5H | 5.8 |
Note：Wearability described in upper table 2 is to scrape wiper heavy burden 5.2kg with 3M to carry out frictional experiment.
The present invention treated modified alta-mud filler can effectively the improve cold coating entirety it can be seen from upper table 2
The characteristics such as wear-resisting, hardness, hence it is evident that improve use quality and the service life of coating entirety, great application value.
Claims (8)
1. a kind of preparation method of the filler of reinforced resin coating intensity, which is characterized in that include the following steps：
（1）Filler cleaning treatment：
Bentonite is first immersed in 8 ~ 10min of processing in salpeter solution, filters out rinsed one time with clear water after the completion, then place into
It is spare that 35 ~ 40min is dried in drying box；
（2）Calcination processing：
By step（1）Treated, and bentonite is put into progress calcination processing in calcining furnace, during which controls the temperature in calcining furnace
It is 800 ~ 860 DEG C, is taken out after 1 ~ 1.5h spare；
（3）It is prepared by modified solution：
A. methyl linoleate and glycerine are put into reaction kettle jointly, be then added its gross mass 1 ~ 3% potassium hydroxide, 1.5
~ 2.5% magnesium hydroxide after being stirred continuously 10 ~ 15min of processing, then alkyl phenol polyoxyethylene ether is added into reaction kettle, simultaneously
The temperature heating of reaction kettle is remained 73 ~ 78 DEG C, and the pressure in reaction kettle is risen into 0.2 ~ 0.3MPa, is stirred continuously processing
Taken out after 40 ~ 45min modification liquid A is spare；
B. by cetyl trimethylammonium bromide and dodecyl sodium sulfate according to weight ratio 2:1 is put into agitator tank jointly,
It is 33 ~ 37 DEG C that heating, which is kept stirring temperature in tank, be stirred continuously after 25 ~ 30min of mixed processing take out modification liquid B is spare；
（4）Modification：
A. by step（2）Treated, and bentonite puts into step（3）It operates in modification liquid A made from a, heating keeps modification liquid
The temperature of A is 55 ~ 60 DEG C, is filtered out after being stirred continuously 40 ~ 45min of processing, is then placed in the environment that temperature is 70 ~ 75 DEG C and does
15 ~ 20min of dry processing, takes out spare after the completion；
B. will operation a treated that bentonite puts into step（3）It operates in modification liquid B made from b, heating keeps modification liquid B
Temperature be 75 ~ 80 DEG C, filtered out after being stirred continuously 20 ~ 25min of processing, it is to be done in 85 ~ 90 DEG C of environment to be then placed in temperature
55 ~ 60min of dry processing takes out after the completion.
2. a kind of preparation method of the filler of reinforced resin coating intensity according to claim 1, which is characterized in that step
（1）Described in salpeter solution in nitric acid mass fraction be 3 ~ 5%.
3. a kind of preparation method of the filler of reinforced resin coating intensity according to claim 1, which is characterized in that step
（1）Described in drying process when control drying box in temperature be 100 ~ 110 DEG C.
4. a kind of preparation method of the filler of reinforced resin coating intensity according to claim 1, which is characterized in that step
（3）It is 2.4 ~ 2.6 to operate the molar ratio that methyl linoleate and glycerine described in a are blended:1.
5. a kind of preparation method of the filler of reinforced resin coating intensity according to claim 1, which is characterized in that step
（3）The addition for operating the alkyl phenol polyoxyethylene ether described in a is the 32 ~ 35% of methyl linoleate gross mass.
6. a kind of preparation method of the filler of reinforced resin coating intensity according to claim 1, which is characterized in that step
（3）It is 800 ~ 900 revs/min to operate the speed of agitator for being stirred processing described in b.
7. a kind of preparation method of the filler of reinforced resin coating intensity according to claim 1, which is characterized in that step
（4）The speed of agitator for operating the stir process described in a is 1500 ~ 1800 revs/min.
8. a kind of preparation method of the filler of reinforced resin coating intensity according to claim 1, which is characterized in that step
（4）The speed of agitator for operating the stir process described in b is 2200 ~ 2500 revs/min.
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| CN112430355A (en) * | 2020-10-29 | 2021-03-02 | 王祥娟 | High-quality elastic rubber and preparation method thereof |
| CN117264506A (en) * | 2023-11-23 | 2023-12-22 | 赛高新材料科技有限公司 | Antibacterial powder coating and preparation method thereof |
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| CN117264506A (en) * | 2023-11-23 | 2023-12-22 | 赛高新材料科技有限公司 | Antibacterial powder coating and preparation method thereof |
| CN117264506B (en) * | 2023-11-23 | 2024-01-26 | 赛高新材料科技有限公司 | Antibacterial powder coating and preparation method thereof |
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Application publication date: 20180720 |
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