A kind of high inorganic filler content laminate surface adhesive plaster and its manufacturing method
【Technical field】
The invention belongs to the technical field of insulating materials, be related to a kind of high inorganic filler content laminate surface adhesive plaster and its
Manufacturing method.
【Background technology】
It is filled out with the development of science and technology needing a large amount of functional inorganic is added in more and more epoxy glass cloth laminated boards
Material.When the content of inorganic filler be more than it is a certain amount of when, the mobility of adhesive plaster will be deteriorated thereon.Add according to original glue formula
Surface adhesive plaster is produced after entering a large amount of inorganic filler, the glass cloth laminated board surface of compacting will appear starved air marks, resin is satisfied
The bad phenomenon of full scale difference, so the resin in the adhesive plaster of surface must have certain mobility.But if only merely pass through
The molding time of adjustment surface glue will appear when then suppressing because of resin stream to improve the mobility of resin in surface sizing cloth
Dynamic fast, filler flows slowly, and the filler accumulation, the floating of uneven color that cause laminate surface water ripples shape occur are bad existing
As.
【Invention content】
It is an object of the invention to overcome the above-mentioned prior art, a kind of high inorganic filler content laminate use is provided
Surface adhesive plaster and its manufacturing method, this method use the addition polyvinyl butyral in epoxy resin to be modified, increase
The strong conjugation of inorganic filler and resin, when solving laminate compacting because in the adhesive plaster of surface resin do not flow due to caused by lack
Glue air marks, resin plumpness difference or caused by resin flows filler accumulation, uneven color floating of water ripples shape etc. it is bad
Phenomenon.
To achieve the goals above, the present invention uses is achieved with technical solution below:
A kind of high inorganic filler content laminate manufacturing method of surface adhesive plaster, includes the following steps:
1) 75~85 parts of organic solvent and 15~25 parts of poly- second are sequentially added in a kettle according to mass fraction meter
Enol butyral simultaneously opens stirring, is then slowly warming up to 55 ± 5 DEG C and keeps the temperature, after polyvinyl butyral all dissolving
It is for use using 80 mesh nylon net filters to butvar adhesive liquid;
2) 10.5~13 parts of organic solvent is added and is mixed in glue kettle, 20~25 parts of epoxy resin, stirring is then added
Uniformly;
3) 32~38 parts of phenolic resin, 9~14 parts of butvar adhesive liquid, 17~22 parts of nothing are sequentially added
Machine filler and 0.5~1 part of benzyl dimethylamine continue to stir the obtained mixture A of 0.5h;
If the molding time of mixture A is measured as 120s-200s at a temperature of (160 ± 2) DEG C with the small skill in using a kitchen knife in cookery, it is further continued for stirring
It mixes 1h and surface glue is made;
If the molding time of mixture A, which is measured at a temperature of (160 ± 2) DEG C with the small skill in using a kitchen knife in cookery, is more than 200s, to mixture A
In add suitable benzyl dimethylamine stirring 0.5h, then detect molding time, until reaching 120~200s, be further continued for stirring 1h
Surface glue is made;
If the molding time of mixture A in (160 ± 2) if DEG C at a temperature of with the small skill in using a kitchen knife in cookery measure be less than 120s, add suitable
0.5h is mixed in epoxy resin, phenolic resin, butvar adhesive liquid and the inorganic filler of amount, then detects molding time until reaching
To 120~200s;
4) surface glue immersion coating is made to surface adhesive plaster on glass cloth.
The present invention, which further improves, to be:
In the step 1), organic solvent a and organic solvent b are toluene, methanol, ethyl alcohol, acetone, methyl acetate, acetic acid
The mixture of any one or two kinds or more in ethyl ester.
In the step 2), organic solvent a and organic solvent b are toluene, methanol, ethyl alcohol, acetone, methyl acetate, acetic acid
The mixture of any one or two kinds or more in ethyl ester.
In the step 1), the acid value of polyvinyl butyral is less than or equal to 0.8mgKOH/g, 20 parts of polyvinyl alcohol contracting fourths
Aldehyde uses 1# flow cup tested viscosities at a temperature of (20 ± 1) DEG C after being dissolved in 80 parts of alcohol solvents be 21~100s.
In the step 2), any one or two kinds or more in epoxy resin E-12, E-20, E-44, E-51
Mixture.
In the step 3), phenolic resin is any one or two kinds in alkalescent phenol resin, acid phenolic resin
Mixture, the wherein amount of solid of phenolic resin are (60 ± 2) %.
In the step 3), inorganic filler is aluminium oxide, aluminium hydroxide, magnesia, magnesium hydroxide, calcium carbonate, titanium dioxide
The mixture of any one or two kinds or more in silicon, titanium dioxide, antimony oxide, di-iron trioxide.
In the step 4), immersion coating is carried out using vertical gluing machine, the oven temperature of vertical gluing machine is 130~
150 DEG C, speed is 5~9m/min.
A kind of high inorganic filler content laminate surface adhesive plaster, surface adhesive plaster glue content 53-56%, soluble resin contain
Measure 85-95%, volatile content<1.0%, fluidity 18-28%.
Compared with prior art, the invention has the advantages that:
Because a certain proportion of poly- present invention employs being added in the epoxy phenolics system of high inorganic filler content
Vinyl butyral is modified, then coordinates suitable mixed glue and photoresist coating process process control, improves high inorganic filler content
Resin system makes film property, resin system and the compatibility of inorganic filler in the adhesive plaster of surface.This manufacturing process both ensure that layer
Larger amount of inorganic filler is added in clamp surface adhesive plaster, and makes the presentation quality of laminate not by the shadow of inorganic filler
It rings.The epoxy glass cloth laminated board surface resin of the high inorganic filler content of adhesive plaster compacting in surface prepared by the present invention is full, has
Gloss, color are uniform, solve poor laminate surface starved air marks, resin plumpness, filler accumulation, uneven color floating etc.
Bad phenomenon.
【Specific implementation mode】
The present invention is described in further detail below:
Embodiment 1
1) butvar adhesive liquid is prepared in a kettle first.
75 parts of solvent a and 25 parts of polyvinyl butyral are sequentially added in a kettle according to mass fraction meter, and
Stirring is started, vapour is then opened and is warming up to (55 ± 5) DEG C, about 8 hours is kept the temperature at such a temperature, waits for that polyvinyl butyral is all molten
It is filtered and packaged after solution for use.
2) and then by formula and defined process surface glue is manufactured.
10.5 parts of solvent b is added according to mass fraction meter and is mixed in glue kettle, 20 parts of epoxy resin is then added, starts
Stirring.
After stir about 0.5h, 38 parts of phenolic resin, 14 parts of butvar adhesive liquid, 17 parts inorganic is added and fills out
Material, 0.5 part of curing accelerator continue to stir 0.5h, and molding time is surveyed in sampling.
It is rear for use to continue stirring 1h or more.
3) glue dipping in surface is finally used to prepare surface adhesive plaster.
Glass cloth is put on by vertical gluing machine operation guide requirement, when oven temperature reaches requirement, glue groove is risen, closes
Upper Extruded roller keeps Extruded roller consistent with the glass cloth direction of motion, scraper is turned over, is tightly attached on Extruded roller, opens adjusting deviation device,
It is allowed to occupy center, opens static eraser, finally start main transmission, adjust glass cloth tension and produced.Adhesive plaster goes out
It should be tested immediately after coming, operator adjusts speed according to test result, and oven temperature not change generally after determining.
Photoresist coating process parameter:130~150 DEG C of oven temperature, speed are 5~9m/min.
Embodiment 2
1) butvar adhesive liquid is prepared in a kettle first.
85 parts of solvent a and 15 parts of polyvinyl butyral are sequentially added in a kettle according to mass fraction meter, and
Stirring is started, vapour is then opened and is warming up to (55 ± 5) DEG C, about 8 hours is kept the temperature at such a temperature, waits for that polyvinyl butyral is all molten
It is filtered and packaged after solution for use.
2) and then by formula and defined process surface glue is manufactured.
10.5 parts of solvent b is added according to mass fraction meter and is mixed in glue kettle, 20 parts of epoxy resin is then added, starts
Stirring.
After stir about 0.5h, 38 parts of phenolic resin, 9 parts of butvar adhesive liquid, 22 parts inorganic is added and fills out
Material, 0.5 part of curing accelerator continue to stir 0.5h, and molding time is surveyed in sampling.
It is rear for use to continue stirring 1h or more.
3) glue dipping in surface is finally used to prepare surface adhesive plaster.
Glass cloth is put on by vertical gluing machine operation guide requirement, when oven temperature reaches requirement, glue groove is risen, closes
Upper Extruded roller keeps Extruded roller consistent with the glass cloth direction of motion, scraper is turned over, is tightly attached on Extruded roller, opens adjusting deviation device,
It is allowed to occupy center, opens static eraser, finally start main transmission, adjust glass cloth tension and produced.Adhesive plaster goes out
It should be tested immediately after coming, operator adjusts speed according to test result, and oven temperature not change generally after determining.
Photoresist coating process parameter:130~150 DEG C of oven temperature, speed are 5~9m/min.
Embodiment 3
1) butvar adhesive liquid is prepared in a kettle first.
75 parts of solvent a and 25 parts of polyvinyl butyral are sequentially added in a kettle according to mass fraction meter, and
Stirring is started, vapour is then opened and is warming up to (55 ± 5) DEG C, about 8 hours is kept the temperature at such a temperature, waits for that polyvinyl butyral is all molten
It is filtered and packaged after solution for use.
2) and then by formula and defined process surface glue is manufactured.
13 parts of solvent b is added according to mass fraction meter and is mixed in glue kettle, 25 parts of epoxy resin is then added, starts to stir
It mixes.
After stir about 0.5h, 32 parts of phenolic resin, 14 parts of butvar adhesive liquid, 17 parts inorganic is added and fills out
Material, 1 part of curing accelerator continue to stir 0.5h, and molding time is surveyed in sampling.
It is rear for use to continue stirring 1h or more.
3) glue dipping in surface is finally used to prepare surface adhesive plaster.
Glass cloth is put on by vertical gluing machine operation guide requirement, when oven temperature reaches requirement, glue groove is risen, closes
Upper Extruded roller keeps Extruded roller consistent with the glass cloth direction of motion, scraper is turned over, is tightly attached on Extruded roller, opens adjusting deviation device,
It is allowed to occupy center, opens static eraser, finally start main transmission, adjust glass cloth tension and produced.Adhesive plaster goes out
It should be tested immediately after coming, operator adjusts speed according to test result, and oven temperature not change generally after determining.
Photoresist coating process parameter:130~150 DEG C of oven temperature, speed are 5~9m/min.
Embodiment 3
1) butvar adhesive liquid is prepared in a kettle first.
85 parts of solvent a and 15 parts of polyvinyl butyral are sequentially added in a kettle according to mass fraction meter, and
Stirring is started, vapour is then opened and is warming up to (55 ± 5) DEG C, about 8 hours is kept the temperature at such a temperature, waits for that polyvinyl butyral is all molten
It is filtered and packaged after solution for use.
2) and then by formula and defined process surface glue is manufactured.
13 parts of solvent b is added according to mass fraction meter and is mixed in glue kettle, 25 parts of epoxy resin is then added, starts to stir
It mixes.
After stir about 0.5h, 32 parts of phenolic resin, 9 parts of butvar adhesive liquid, 22 parts inorganic is added and fills out
Material, 1 part of curing accelerator continue to stir 0.5h, and molding time is surveyed in sampling.
It is rear for use to continue stirring 1h or more.
3) glue dipping in surface is finally used to prepare surface adhesive plaster.
Glass cloth is put on by vertical gluing machine operation guide requirement, when oven temperature reaches requirement, glue groove is risen, closes
Upper Extruded roller keeps Extruded roller consistent with the glass cloth direction of motion, scraper is turned over, is tightly attached on Extruded roller, opens adjusting deviation device,
It is allowed to occupy center, opens static eraser, finally start main transmission, adjust glass cloth tension and produced.Adhesive plaster goes out
It should be tested immediately after coming, operator adjusts speed according to test result, and oven temperature not change generally after determining.
Photoresist coating process parameter:130~150 DEG C of oven temperature, speed are 5~9m/min.
The surface glue that is blended according to embodiment 1, embodiment 2, embodiment 3 and embodiment 4, surface adhesive plaster index
Test and the high inorganic filler content epoxy glass cloth laminated board surface condition such as the following table 1 finally suppressed:
Table 1:Surface glue, surface adhesive plaster index test and the laminate surface situation finally suppressed
The above content is merely illustrative of the invention's technical idea, and protection scope of the present invention cannot be limited with this, every to press
According to technological thought proposed by the present invention, any change done on the basis of technical solution each falls within claims of the present invention
Protection domain within.