CN110172165A - A kind of preparation method of silica-filled polytetrafluoroethyldispersion dispersion - Google Patents
A kind of preparation method of silica-filled polytetrafluoroethyldispersion dispersion Download PDFInfo
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- CN110172165A CN110172165A CN201910513664.0A CN201910513664A CN110172165A CN 110172165 A CN110172165 A CN 110172165A CN 201910513664 A CN201910513664 A CN 201910513664A CN 110172165 A CN110172165 A CN 110172165A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2327/18—Homopolymers or copolymers of tetrafluoroethylene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K3/36—Silica
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Abstract
The present invention provides a kind of preparation method of silica-filled polytetrafluoroethyldispersion dispersion, the present invention carries out dispersion mixing by filler and polytetrafluoroethylene (PTFE) in liquid medium, incorporation time and operation difficulty are mixed far below conventional solid powder, and can be used for impregnation technology；By the dispersion liquid, the interface binding power of filler and polytetrafluoroethylene (PTFE) is improved, the surface defect in dipping process is improved；The present invention is highly suitable for impregnated glass colth, to produce high performance copper-clad polytetrafluoroethylplate plate；The disadvantages such as the existing copper-clad plate thermal expansion coefficient of effective solution is big, wear no resistance, mechanical strength is low, improve inorganic filler sedimentation problem, significantly improve glue composition homogeneity, this method passes through steric hindrance and electrical charge rejection effect, so that mutually exclusive between filler particles, extend particle suspension time, guarantees dispersion consistency.
Description
Technical field
The invention belongs to the preparation methods of polytetrafluoroethyldispersion dispersion, and in particular to silica-filled polytetrafluoroethylene (PTFE) point
The preparation method of dispersion liquid.
Background technique
Polytetrafluoroethylene (PTFE) has excellent chemical stability and dielectric properties, can be used for the production of high-frequency copper-clad plate.But because
The disadvantages such as its thermal expansion coefficient is big, wear no resistance, mechanical strength is low, so that copper-clad plate poor in processability, limits it and further answer
With, in order to improve the processability of copper-clad plate, solved by way of adding inorganic filler into polytetrafluoroethylene (PTFE) in the industry, it is main
Want method be solid polytetrafluor ethylene and inorganic filler mixed after be sintered, then cut into film, carry out it is folded match, hot pressing
At plate, the method principle is simple, but operation difficulty is big, high to equipment material and required precision, and plate is without reinforcement materials for support,
Mechanical strength is not high.The present invention prepares a kind of polytetrafluoroethyldispersion dispersion of modification, and filler and polytetrafluoroethylene (PTFE) is made to be situated between in liquid
Dispersion mixing, incorporation time and operation difficulty are carried out in matter to mix far below conventional solid powder, and can be used for impregnated glass colth,
To produce high performance copper-clad polytetrafluoroethylplate plate.
Summary of the invention
It is high to equipment material and required precision the purpose of the present invention is to overcome prior art operation difficulty big, and plate
Without reinforcement materials for support, the disadvantages of mechanical strength is not high.A kind of preparation of silica-filled polytetrafluoroethyldispersion dispersion is provided
Method makes filler and polytetrafluoroethylene (PTFE) carry out dispersion mixing, incorporation time and operation difficulty in liquid medium far below tradition
Solid powder mixing, and can be used for impregnation technology, by the dispersion liquid, the interface binding power of filler and polytetrafluoroethylene (PTFE) is improved,
The surface defect in dipping process is improved, and by steric hindrance and electrical charge rejection effect, so that mutually arranging between filler particles
Reprimand extends particle suspension time, guarantees that dispersion consistency significantly improves glue by improving inorganic filler sedimentation problem
Compositional uniformity.
The technical scheme adopted by the invention is that:
A kind of preparation method of silica-filled polytetrafluoroethyldispersion dispersion includes the following steps:
Step 1 production dispersion liquid A:a. weighs the polytetrafluoroethyldispersion dispersion (decentralized medium that 100 parts of solid contents are 60%
For water), it pours into 1# constant temperature stirred tank and is stirred, 20~25 DEG C of set temperature, 300~600rpm of mixing speed；B. to 1#
Glacial acetic acid is added in stirred tank, and stand-by dispersion liquid A is made；
Step 2 makes mixed liquid B: fused silica powder (D50≤5 μm, D100≤10 μm) are added planetary a.
In ball mill；B. a container is separately taken, by dimethyl maleate ammonium salt and polyisocyanate methyl esters, deionized water is added and is uniformly mixed,
Mixed liquid B is made；
Step 3 makes slurry C: mixed liquid B being poured into planetary ball mill, ball mill is opened, sets spin velocity
600~800rpm, revolution 200~400rpm of angular speed carry out grinding 2~3 hours, and slurry C is made；
Step 4 makes dispersion liquid D:a. and deionized water is added in 2# constant temperature stirred tank, and 20~25 DEG C of set temperature, stirring
300~600rpm of speed；B. it is poured slowly into slurry C into 2# stirred tank, stirs 30~60min, dispersion liquid D is made；
Step 5 makes polytetrafluoroethyldispersion dispersion: dispersion liquid D is slowly added in 1# stirred tank by a., maintains stirring kettle temperature
Degree and revolving speed are constant, while adding glacial acetic acid thereto to maintain dispersion liquid pH value in 5~7 ranges, continue to stir after the completion
30~60min；B. polypropylene ester and poly- 2- methylsiloxane are added into 1# stirred tank, continue 30~60min of stirring, it is final to make
Obtain polytetrafluoroethyldispersion dispersion.
The step 1 makes dispersion liquid A: after adding glacial acetic acid into 1# stirred tank, adjusting dispersion liquid pH value in 5~7 models
In enclosing.
The step 2 makes mixed liquid B: the fused silica powder that a. is added into planetary ball mill is 50~70
Part；B. weighed dimethyl maleate ammonium salt is 0.5~2 part, and 1~3 part of polyisocyanate methyl esters, the deionized water of addition is 5~8
Part.
The step 3 makes slurry C: the deionized water being added in 2# constant temperature stirred tank is 30~50 parts.
The step 5 makes polytetrafluoroethyldispersion dispersion: the polypropylene ester and poly- 2- methyl silicon added into 1# stirred tank
Oxygen alkane is 0.1~0.6 part.
The step 5 makes polytetrafluoroethyldispersion dispersion: polytetrafluoroethyldispersion dispersion need to seal under the conditions of 20~25 DEG C
Storage.
Beneficial effect
1, the dispersion liquid substitutes existing epoxy glue aqueous systems, adapts to existing copper-clad plate production technology；
2, inorganic filler sedimentation problem is improved, glue composition homogeneity is significantly improved, inorganic filler particle cannot be molten
Xie Yushui is precipitated after reuniting, and causes dispersion liquid is uniform to sexually revise, and this method is made by steric hindrance and electrical charge rejection effect
It is mutually exclusive between filler particles, extend particle suspension time, guarantee dispersion consistency；
3, inorganic filler is different from the surface tension of medium water, easily forms " flake ", " starved " etc. in surface of semi-finished and lacks
It falls into, and the nonflowing character of polytetrafluoroethylene (PTFE) causes hot pressing process, and such defect cannot diminish, by the use of the dispersion liquid,
Surface tension is reduced, levelability is improved.
Specific embodiment
Below in conjunction with example, the present invention is described further:
A kind of preparation method of silica-filled polytetrafluoroethyldispersion dispersion includes the following steps:
Step 1 production dispersion liquid A:a. weighs the polytetrafluoroethyldispersion dispersion (decentralized medium that 100 parts of solid contents are 60%
For water), it pours into 1# constant temperature stirred tank and is stirred, 20~25 DEG C of set temperature, 300~600rpm of mixing speed；B. to 1#
Glacial acetic acid is added in stirred tank, and stand-by dispersion liquid A is made；
Step 2 makes mixed liquid B: fused silica powder (D50≤5 μm, D100≤10 μm) are added planetary a.
In ball mill；B. a container is separately taken, by dimethyl maleate ammonium salt and polyisocyanate methyl esters, deionized water is added and is uniformly mixed,
Mixed liquid B is made；
Step 3 makes slurry C: mixed liquid B being poured into planetary ball mill, ball mill is opened, sets spin velocity
600~800rpm, revolution 200~400rpm of angular speed carry out grinding 2~3 hours, and slurry C is made；
Step 4 makes dispersion liquid D:a. and deionized water is added in 2# constant temperature stirred tank, and 20~25 DEG C of set temperature, stirring
300~600rpm of speed；B. it is poured slowly into slurry C into 2# stirred tank, stirs 30~60min, dispersion liquid D is made；
Step 5 makes polytetrafluoroethyldispersion dispersion: dispersion liquid D is slowly added in 1# stirred tank by a., maintains stirring kettle temperature
Degree and revolving speed are constant, while adding glacial acetic acid thereto to maintain dispersion liquid pH value in 5~7 ranges, continue to stir after the completion
30~60min；B. polypropylene ester and poly- 2- methylsiloxane are added into 1# stirred tank, continue 30~60min of stirring, it is final to make
Obtain polytetrafluoroethyldispersion dispersion.
Preferably, in production dispersion liquid A: after adding glacial acetic acid into 1# stirred tank, adjusting dispersion liquid pH value 5~7
In range.
Preferably, production mixed liquid B in: the fused silica powder that a. is added into planetary ball mill be 50~
70 parts；B. weighed dimethyl maleate ammonium salt is 0.5~2 part, and 1~3 part of polyisocyanate methyl esters, the deionized water of addition is 5
~8 parts.
Preferably, in production slurry C: the deionized water being added in 2# constant temperature stirred tank is 30~50 parts.
Preferably, in production polytetrafluoroethyldispersion dispersion: the polypropylene ester and poly- 2- methyl added into 1# stirred tank
Siloxanes is 0.1~0.6 part.
Preferably, after making polytetrafluoroethyldispersion dispersion: polytetrafluoroethyldispersion dispersion need to be close under the conditions of 20~25 DEG C
Seal storage up for safekeeping.
The present invention carries out dispersion mixing by filler and polytetrafluoroethylene (PTFE) in liquid medium, and incorporation time and operation are difficult
Degree is mixed far below conventional solid powder, and can be used for impregnation technology.
The present invention is improved the interface binding power of filler and polytetrafluoroethylene (PTFE) by the dispersion liquid, improved in dipping process
Surface defect.
The present invention is highly suitable for impregnated glass colth, to produce high performance copper-clad polytetrafluoroethylplate plate.
Present invention improves inorganic filler sedimentation problems, glue composition homogeneity are significantly improved, due to inorganic filler
Grain cannot be dissolved in water, precipitate after reuniting, cause dispersion liquid is uniform to sexually revise, and this method passes through steric hindrance and electrical charge rejection
Effect, so that it is mutually exclusive between filler particles, extend particle suspension time, guarantees dispersion consistency.
Using technical solutions according to the invention or those skilled in the art under the inspiration of technical solution of the present invention,
Similar technical solution is designed, and reaches above-mentioned technical effect, is to fall into protection scope of the present invention.
Claims (6)
1. a kind of preparation method of silica-filled polytetrafluoroethyldispersion dispersion, it is characterised in that: described silica-filled
The preparation method of polytetrafluoroethyldispersion dispersion includes the following steps:
Step 1 production dispersion liquid A:a. weighs the polytetrafluoroethyldispersion dispersion that 100 parts of solid contents are 60%, and (decentralized medium is
Water), it pours into 1# constant temperature stirred tank and is stirred, 20~25 DEG C of set temperature, 300~600rpm of mixing speed；B. it is stirred to 1#
It mixes and adds glacial acetic acid in kettle, stand-by dispersion liquid A is made；
Step 2 makes mixed liquid B: planetary type ball-milling is added in fused silica powder (D50≤5 μm, D100≤10 μm) by a.
In machine；B. a container is separately taken, by dimethyl maleate ammonium salt and polyisocyanate methyl esters, deionized water is added and is uniformly mixed, is made
Mixed liquid B；
Step 3 makes slurry C: mixed liquid B poured into planetary ball mill, unlatching ball mill, setting spin velocity 600~
800rpm, revolution 200~400rpm of angular speed carry out grinding 2~3 hours, and slurry C is made；
Step 4 makes dispersion liquid D:a. and deionized water is added in 2# constant temperature stirred tank, and 20~25 DEG C of set temperature, mixing speed
300~600rpm；B. it is poured slowly into slurry C into 2# stirred tank, stirs 30~60min, dispersion liquid D is made；
Step 5 make polytetrafluoroethyldispersion dispersion: dispersion liquid D is slowly added in 1# stirred tank by a., maintain stirred tank temperature and
Revolving speed is constant, at the same thereto add glacial acetic acid to maintain dispersion liquid pH value in 5~7 ranges, continue after the completion stirring 30~
60min；B. polypropylene ester and poly- 2- methylsiloxane are added into 1# stirred tank, continue 30~60min of stirring, it is final to be made poly-
Tetrafluoroethene dispersion liquid.
2. the preparation method of silica-filled polytetrafluoroethyldispersion dispersion as described in claim 1, it is characterised in that: the step
Rapid 1 production dispersion liquid A: after adding glacial acetic acid into 1# stirred tank, dispersion liquid pH value is adjusted in 5~7 ranges.
3. the preparation method of silica-filled polytetrafluoroethyldispersion dispersion as described in claim 1, it is characterised in that: described
Step 2 makes mixed liquid B: the fused silica powder that a. is added into planetary ball mill is 50~70 parts；B. weighed
Dimethyl maleate ammonium salt is 0.5~2 part, and 1~3 part of polyisocyanate methyl esters, the deionized water of addition is 5~8 parts.
4. the preparation method of silica-filled polytetrafluoroethyldispersion dispersion as described in claim 1, it is characterised in that: described
Step 3 makes slurry C: the deionized water being added in 2# constant temperature stirred tank is 30~50 parts.
5. the preparation method of silica-filled polytetrafluoroethyldispersion dispersion as described in claim 1, it is characterised in that: described
Step 5 makes polytetrafluoroethyldispersion dispersion: the polypropylene ester and poly- 2- methylsiloxane added into 1# stirred tank be 0.1~
0.6 part.
6. the preparation method of silica-filled polytetrafluoroethyldispersion dispersion as described in claim 1, it is characterised in that: described
Step 5 make polytetrafluoroethyldispersion dispersion: polytetrafluoroethyldispersion dispersion need under the conditions of 20~25 DEG C sealed storage.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910513664.0A CN110172165A (en) | 2019-06-14 | 2019-06-14 | A kind of preparation method of silica-filled polytetrafluoroethyldispersion dispersion |
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| CN201910513664.0A CN110172165A (en) | 2019-06-14 | 2019-06-14 | A kind of preparation method of silica-filled polytetrafluoroethyldispersion dispersion |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113604099A (en) * | 2021-07-08 | 2021-11-05 | 江苏海田电子材料有限公司 | Low-dielectric-constant solder resist ink and preparation method thereof |
| CN114161741A (en) * | 2021-12-06 | 2022-03-11 | 中国电子科技集团公司第四十六研究所 | Method for forming polytetrafluoroethylene impregnated sheet with high filler content |
-
2019
- 2019-06-14 CN CN201910513664.0A patent/CN110172165A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113604099A (en) * | 2021-07-08 | 2021-11-05 | 江苏海田电子材料有限公司 | Low-dielectric-constant solder resist ink and preparation method thereof |
| CN114161741A (en) * | 2021-12-06 | 2022-03-11 | 中国电子科技集团公司第四十六研究所 | Method for forming polytetrafluoroethylene impregnated sheet with high filler content |
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Application publication date: 20190827 |