CN109826051A - A kind of single-component water-based organosilicon paper mould release and preparation method thereof - Google Patents
A kind of single-component water-based organosilicon paper mould release and preparation method thereof Download PDFInfo
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- CN109826051A CN109826051A CN201910045695.8A CN201910045695A CN109826051A CN 109826051 A CN109826051 A CN 109826051A CN 201910045695 A CN201910045695 A CN 201910045695A CN 109826051 A CN109826051 A CN 109826051A
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Abstract
The invention discloses a kind of single-component water-based organosilicon paper mould releases, it is characterized in that, by weight percentage, including following component: siloxanyl monomers 5%~60%, cationic emulsifier 1%~10%, catalyst 0.1%~2%, stabilizer 1%~10%, dispersing agent 1%~10%, crosslinking agent 0.1%~20%, neutralizer 0.1%~3%, deionized water 10%~90%.The invention also discloses preparation methods.The present invention, which is formed by release film, a preferable peeling force and aging peeling force, surfacing, so that paper jaundice is become fragile discoloration, can write, can long-term preservation；And single-component product is lower to the skill requirement of construction, is easier to construct.
Description
Technical field
The invention belongs to organosilicon paper mould release preparation fields, and in particular to a kind of single-component water-based organosilicon paper from
Type agent and preparation method thereof.
Background technique
Paper mould release is applied to the paper such as Ge Laxin paper and paper, U.S. line paper, art paper, heat-sensitive paper, separate paper, these
Paper side coats adhesive (such as white glue with vinyl, hot melt adhesive etc.), forms adhesive-layer, and another side coating release agent forms release film.
Release film is bonded adhesive-layer, can protect adhesive-layer, be contaminated it not before pasting, and will not lose its viscosity, and viscose glue
When layer is from release film stripping, flying chip will not be generated, the physical property of adhesive-layer will not be injured.
The paper mould release used on the market at present, mainly following two:
First is that solvent-based two-component silicone release agent, main ingredient is Methyl Hydrogen Polysiloxane Fluid, vinyl silicone oil, catalyst
Chloroplatinic acid, volatile solvent (such as toluene, gasoline, isopropanol, acetone), it is inflammable and explosive because containing a large amount of solvent, to environment
It will cause very big injury with human body, 120 DEG C~160 DEG C of solidification temperature；
Another is aqueous double-component organic silicon emulsion, and main component is Methyl Hydrogen Polysiloxane Fluid, vinyl silicone oil, catalysis
Agent chloroplatinic acid, emulsifier, deionized water are water-based emulsion, and solvent-free release, to human body and environmentally friendly, solidification temperature is general
It is 100 DEG C~130 DEG C.
The curing mechanism of two kinds of mould releases is all Methyl Hydrogen Polysiloxane Fluid and vinyl silicone oil in catalyst chloroplatinic acid and reaction
At temperature (and solidification temperature), hydrosilylation occurs, the polysiloxanes of cross-linked structure is generated in paper surface, because solid
It is relatively high to change temperature, easily turns yellow embrittlement so generating greatly injury, paper to paper, quick aging is unable to long-term preservation.
Especially heat-sensitive paper, when being placed in 70 DEG C or more of environment, the writing shown on heat-sensitive paper is unstable, easy recession,
Content is difficult to recognize.When being placed in 100 DEG C or more of environment, heat-sensitive paper can complete blackening.And at the construction field (site), two-component produces
Product, which need to weigh, to be counted, and is easily caused complicated for operation and product unstable, is increased difficulty of construction.
Summary of the invention
In order to overcome the drawbacks described above of the prior art, an object of the present invention is to provide a kind of single-component water-based organosilicon
Paper mould release.
The second object of the present invention is to provide a kind of preparation method of single-component water-based organosilicon paper mould release.
One of in order to achieve the object of the present invention, used technical solution is:
A kind of single-component water-based organosilicon paper mould release, by weight percentage, including following component:
Siloxanyl monomers 5%~60%,
Cationic emulsifier 1%~10%,
Catalyst 0.1%~2%,
Stabilizer 1%~10%,
Dispersing agent 1%~10%,
Crosslinking agent 0.1%~20%,
Neutralizer 0.1%~3%,
Deionized water 10%~90%.
In a preferred embodiment of the invention, the siloxanyl monomers include octamethylcy-clotetrasiloxane D4, ring
In the mixture D MC (including hexamethyl cyclotrisiloxane, octamethylcy-clotetrasiloxane and decamethylcyclopentaandoxane) of siloxanes
Any one or two kinds.
In a preferred embodiment of the invention, the cationic emulsifier includes dodecyl dimethyl benzyl bromide
Change ammonium, dodecyl benzyl dimethyl ammonium chloride, dodecyl trimethyl ammonium bromide, dodecyl trimethyl ammonium chloride, 16
Alkyl trimethyl ammonium bromide, hexadecyltrimethylammonium chloride, octadecyl dimethyl benzyl ammonium bromide, octadecyldimethyl
Benzyl ammonium chloride, octadecyltrimethylammonium chloride, any one or more in didodecyldimethylammbromide bromide.
In a preferred embodiment of the invention, the catalyst is alkali metal hydroxide, preferably lithium hydroxide,
Any one or more in sodium hydroxide, potassium hydroxide.
In a preferred embodiment of the invention, the stabilizer includes fatty alcohol polyoxyethylene ether paregal O system
It is any during column, fatty alcohol polyoxyethylene ether AEO series, polyethylene glycol PEG series, collateralization isomeric alcohol polyethenoxy ether are serial
It is one or more.
In a preferred embodiment of the invention, the dispersing agent is WA, that is, fatty alcohol polyoxyethylene ether methyl silicon
Alkane.
In a preferred embodiment of the invention, the crosslinking agent includes silane coupling agent, as tetramethoxy-silicane,
Tetraethoxysilane, methyltrimethoxysilane, methyltriethoxysilane, ethyl trimethoxy silane, n-propyl trimethoxy
Base silane, n-propyl triethoxysilane, isobutyl triethoxy silane, n-hexyl trimethoxy silane, three ethoxy of n-hexyl
Base silane, n-octyl trimethoxy silane, n-octytriethoxysilane, isooctyltriethoxysilane, positive decyl trimethoxy
Base silane, dodecyltrimethoxysilane, dodecyl triethoxysilane, hexadecyl trimethoxy silane, dimethyl
Dimethoxysilane, 3- aminopropyl trimethoxy siloxane, 3- aminopropyl triethoxysilane, 3- aminopropyltriethoxy diethoxy
Silane, N- (β-aminoethyl-γ-aminopropyl) methyl dimethoxysilane, N- (β-aminoethyl-γ-aminopropyl) trimethoxy silicon
Alkane, N- phenyl amino propyl trimethoxy silane, 3- diethylin propyl trimethoxy silicane, n-butyl amine base propyl trimethoxy
Silane, diethylenetriamine base propyl trimethoxy silicane, any one or more in 3- urea propyl trimethoxy silicane.
In a preferred embodiment of the invention, the neutralizer includes acetic acid, in phosphoric acid any one or it is more
Kind.
In order to achieve the object of the present invention two, used technical solution is as follows:
A kind of preparation method of single-component water-based organosilicon paper mould release, includes the following steps:
Step 1: by stabilizer, partial cation emulsifier, siloxanyl monomers, crosslinking agent is add to deionized water, mixed
Conjunction stirs evenly, and crosses homogenizer (20MPa~50MPa) once, obtains pre-emulsion A；
Step 2: by remaining cationic emulsifier, catalyst, dispersing agent, deionized water, the pre-emulsion A, addition is instead
It answers in kettle, is mixed evenly, be warming up to 60 DEG C~90 DEG C, insulation reaction 5h~12h；
Step 3: being cooled to 15 DEG C~40 DEG C, and neutralizer is added and adjusts pH value to 6~7, obtains blue-fluorescence lotion, i.e.,
For single-component water-based organosilicon paper mould release.
The beneficial effects of the present invention are:
The present invention, which is formed by release film, preferable peeling force and aging peeling force, and surfacing does not make paper turn to be yellow
Become fragile discoloration, can write, can long-term preservation；
And single-component product is lower to the skill requirement of construction, is easier to construct.
Detailed description of the invention
Fig. 1 is the heat-sensitive paper (65 DEG C of solidification temperature, curing time 10s) of single-component water-based organosilicon paper mould release coating
Schematic diagram.
Fig. 2 be the coating of double-component aqueous organosilicon paper mould release heat-sensitive paper (115 DEG C of solidification temperature, curing time
Schematic diagram 10s).
Specific embodiment
The principle of the invention lies in:
The single-component water-based organosilicon paper mould release of this product is organic silicon monomer and crosslinking agent in catalyst and fire-bar
Under part, open loop and dealcoholization occurs, generates a kind of polysiloxane polymer of cross-linked structure.Mould release using water as dispersing agent,
Solvent-free volatilization, it is harmless to environment and human body, it can adjust peeling force and aging peeling force, and be one-component lotion, construction party
Just, it is ensured that the stability of product quality.When mould release be coated in paper on, be heated to 55 DEG C~90 DEG C, time 10s~20s,
It will form the polysiloxane film of one layer of fine and close reticular structure in paper surface, this film surface is smooth, smooth, transparency
Height, chemical property are stablized, and heat-resistant pressure-resistant, elasticity is good, and hydrophobicity is good, can write, therefore can be widely used for the paper of multiple fields.
Based on the above principles, the present invention is explained further further according to specific embodiment below:
Embodiment 1
By 0.6 gram of paregal O -20,0.6 gram of TO-10,2.9 grams of dodecyl dimethyl benzyl ammonium bromide, octadecyl
2.1 grams of dimethylbenzyl ammonium bromide, 60 grams of D4,1.5 grams of ethyl trimethoxy silane, 3- aminopropyl trimethoxy siloxane 1.2
Gram, it 60 grams of deionized water, is mixed evenly, homogenizer 30MPa excessively is primary, obtains pre-emulsion A.
In equipped with blender, the three-necked flask for flowing back condenser, thermometer, dodecyl dimethyl Benzylphosphonium Bromide is added
2.9 grams of ammonium, 2.1 grams of octadecyl dimethyl benzyl ammonium bromide, 1.5 grams of KOH, 2.4 grams of WA, 66.6 grams of deionized water, step 1
128.9 grams of the pre-emulsion A of preparation, is mixed evenly, and is warming up to 80 ± 2 DEG C, insulation reaction 5h.
It is cooled to room temperature, 4.6 grams of acetic acid is added, is adjusted to pH value 6.5, obtains the blue-fluorescence of organosilicon solid content 30%
Cation emulsion mould release.
By adjusting release agent prescription component selection, each component mass ratio design, reaction time and reaction temperature
Etc. one or several kinds, the present invention can derive multiple and different embodiments, obtain peeling force of different sizes and aging removing
Power does not enumerate herein to be suitable for the paper in various fields and industry, is selected below with list mode representative
Wherein several embodiments the present invention is further illustrated.
On the basis of embodiment 1, by mould release each component mass ratio (catalyst, crosslinking agent), reaction temperature, anti-
Adjusting between seasonable, obtains the mould release of different peeling forces and aging peeling force.All embodiments are by 1,2,3 3 steps
Be made, above three step divided by lower adjustment outside, with embodiment 1 the step of it is identical.It is each by each list of steps explanation below
The manufacture craft of embodiment:
Table 1: step 1
Table 2: step 2 and 3
Comparative example 1
In the there-necked flask that blender, reflux condenser, thermometer are housed, 200 grams of DMC are added, high containing hydrogen silicone oil
It (202) 164.7 grams, 7.3 grams of the catalyst concentrated sulfuric acid, is mixed evenly, is warming up to 55 ± 5 DEG C, 7 hours of insulation reaction are delayed
It is slow to be added 8 grams of neutralizer sodium carbonate, it is sufficiently stirred and is neutralized to reaction solution and is in neutrality, filter, low-boiling-point substance is sloughed in vacuum distillation, is obtained
Colorless and transparent Methyl Hydrogen Polysiloxane Fluid, hydrogen content 0.7%, viscosity 120CS.
31.8 grams of the Methyl Hydrogen Polysiloxane Fluid of step 1,150 grams of vinyl silicone oil (contents of ethylene 2%, viscosity 1000cS),
It 8 grams of fatty alcohol polyoxyethylene ether AEO-9,1,303 10 grams of isomerous tridecanol polyoxyethylene ether, is added in reaction kettle, is mixed
Uniformly, using high-speed shearing emulsion machine, 60 grams of deionized waters is persistently added dropwise, time for adding 15 minutes, are eventually adding deionized water
It 344.7 grams, 1.5 grams of glacial acetic acid, stirs evenly, adjusting pH value is 6, obtains milky component A lotion, solid content 30%.
1 gram of chloroplatinic acid, 100 grams of vinyl silicone oil (contents of ethylene 1%, viscosity 500cS), fatty alcohol polyoxyethylene ether
(AEO-9) it 5 grams, 1,303 5 grams of isomerous tridecanol polyoxyethylene ether, is added in reaction kettle, is mixed evenly, using cutting at a high speed
Mulser is cut, 33 grams of deionized water is persistently added dropwise, time for adding 15 minutes, is eventually adding 192.7 grams of deionized water, acetic acid 0.5
Gram, it stirs evenly, adjusting pH value is 6, as milky B component lotion, solid content 30%.
Comparative example 2
In the there-necked flask that blender, reflux condenser, thermometer are housed, 200 grams of DMC are added, high containing hydrogen silicone oil
It (202) 48 grams, 2.1 grams of hexamethyldisiloxane, 5 grams of the catalyst concentrated sulfuric acid, is mixed evenly, is warming up to 55 ± 5 DEG C, heat preservation
7 hours are reacted, are slowly added to 5.5 grams of neutralizer sodium carbonate, according to the operating procedure of the step 1 in comparative example 1, are made colourless
Transparent Methyl Hydrogen Polysiloxane Fluid, hydrogen content 0.3%, viscosity 200CS.
By 66 grams of above-mentioned Methyl Hydrogen Polysiloxane Fluid, 115.8 grams of vinyl silicone oil (contents of ethylene 2%, viscosity 1000cS), second
9 grams of alkenyl silicone oil (contents of ethylene 1%, viscosity 500cS), is mixed evenly by 415.2 grams of toluene, be oiliness organosilicon from
Type agent component A.
It 1 gram of chloroplatinic acid, 337 grams of isopropanol, is uniformly mixed, is B component.
Comparative test:
The mould release of example 1~8 and comparative example 1~2 is subjected to physical characteristic measurement, related data test method is as follows:
Peeling force
White glue with vinyl is applied to the one side of release paper using scraper for coating method, coating layer thickness is 8 μm, by each mould release be applied to from
The another side (A:B component is mixed according to the mass ratio of 20:1 in comparative example) of type paper, coating layer thickness is 3 μm, release by what is coated
Paper is placed in baking oven, and the release paper of Examples 1 to 8 sets solidification temperature as 70 DEG C ± 6 DEG C, time 10s, comparative example 1 and 2 from
Type paper sets 120 ± 5 DEG C of solidification temperature, time 10s.Mucilage glue surface after taking-up according to a piece of paper is close to the layer upper surface of another a piece of paper
Order superposition, paper number are 200, and by the paper merging press machine of superposition, pressure is set as 10~30Mpa, time 0.75
A hour is cut into the batten of 30mm wide along longitudinal direction after taking-up.
With 180 ° of peel angle, the peeling rate of 300mm/min carries out the test of peeling force.Every kind of sample measurement 5
It is secondary, it is averaged.
Aging peeling force and texture of paper variation:
The batten of above-mentioned 30mm wide is placed in baking oven, 70 ± 5 DEG C of set temperature, 120 hours of time.Batten is taken out,
With 180 ° of peel angle, the peeling rate of 300mm/min carries out the test of peeling force, and observes the variation of texture of paper.Often
Kind sample measures 5 times, is averaged,
Measurement data is shown in Table 3: peeling force indicates with g/inch,
Table 3
According to table 3, the embodiment of the present invention, which is formed by release film, preferable peeling force and aging peeling force, surface
It is smooth, so that paper jaundice is become fragile discoloration, can write, it can long-term preservation.
By Fig. 1 and Fig. 2 comparison it is found that the release film of the embodiment of the present invention for heat-sensitive paper when using, Neng Gouyou
Effect prevents heat-sensitive paper from blacking.
Claims (9)
1. a kind of single-component water-based organosilicon paper mould release, which is characterized in that by weight percentage, including following component:
Siloxanyl monomers 5%~60%,
Cationic emulsifier 1%~10%,
Catalyst 0.1%~2%,
Stabilizer 1%~10%,
Dispersing agent 1%~10%,
Crosslinking agent 0.1%~20%,
Neutralizer 0.1%~3%,
Deionized water 10%~90%.
2. a kind of single-component water-based organosilicon paper mould release as described in claim 1, which is characterized in that the siloxanes
Monomer includes mixture D MC (including the hexamethyl cyclotrisiloxane, prestox ring of octamethylcy-clotetrasiloxane D4, cyclosiloxane
Tetrasiloxane and decamethylcyclopentaandoxane) in any one or two kinds.
3. a kind of single-component water-based organosilicon paper mould release as described in claim 1, which is characterized in that the cation
Emulsifier includes dodecyl dimethyl benzyl ammonium bromide, dodecyl benzyl dimethyl ammonium chloride, trimethyl bromine
Change ammonium, dodecyl trimethyl ammonium chloride, cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride, octadecyl
Dimethylbenzyl ammonium bromide, stearyl dimethyl benzyl ammonium chloride, octadecyltrimethylammonium chloride, double dimethyls
Any one or more in base ammonium bromide.
4. a kind of single-component water-based organosilicon paper mould release as described in claim 1, which is characterized in that the catalyst
It is alkali metal hydroxide.
5. a kind of single-component water-based organosilicon paper mould release as described in claim 1, which is characterized in that the stabilizer
Including fatty alcohol polyoxyethylene ether paregal O series, fatty alcohol polyoxyethylene ether AEO series, polyethylene glycol PEG series, branch
Change any one or more in isomeric alcohol polyethenoxy ether series.
6. a kind of single-component water-based organosilicon paper mould release as described in claim 1, which is characterized in that the dispersing agent
For WA, that is, fatty alcohol polyoxyethylene ether methyl-monosilane.
7. a kind of single-component water-based organosilicon paper mould release as described in claim 1, which is characterized in that the crosslinking agent
Including silane coupling agent, as tetramethoxy-silicane, tetraethoxysilane, methyltrimethoxysilane, methyltriethoxysilane,
Ethyl trimethoxy silane, n-propyl trimethoxy silane, n-propyl triethoxysilane, isobutyl triethoxy silane, just
Hexyl trimethoxysilane, n-hexyl triethoxysilane, n-octyl trimethoxy silane, it is n-octytriethoxysilane, different
Octyltri-ethoxysilane, positive decyl trimethoxy silane, dodecyltrimethoxysilane, dodecyl triethoxysilicane
Alkane, hexadecyl trimethoxy silane, dimethyldimethoxysil,ne, 3- aminopropyl trimethoxy siloxane, 3- aminopropyl three
Ethoxysilane, 3- aminopropyltriethoxy diethoxy silane, N- (β-aminoethyl-γ-aminopropyl) methyl dimethoxysilane, N-
(β-aminoethyl-γ-aminopropyl) trimethoxy silane, N- phenyl amino propyl trimethoxy silane, 3- diethylin propyl three
Methoxy silane, n-butyl amine base propyl trimethoxy silicane, diethylenetriamine base propyl trimethoxy silicane, 3- urea propyl front three
Any one or more in oxysilane.
8. a kind of single-component water-based organosilicon paper mould release as described in claim 1, which is characterized in that the neutralizer
Any one or more including acetic acid, in phosphoric acid.
9. a kind of preparation side of single-component water-based organosilicon paper mould release as described in any one of working as claim 1-8
Method, which comprises the steps of:
Step 1: by stabilizer, partial cation emulsifier, siloxanyl monomers, crosslinking agent is add to deionized water, and mixing is stirred
It mixes uniformly, crosses homogenizer (20MPa~50MPa) once, obtain pre-emulsion A；
Step 2: by remaining cationic emulsifier, catalyst, dispersing agent, deionized water, the pre-emulsion A, addition reaction kettle
In, it is mixed evenly, is warming up to 60 DEG C~90 DEG C, insulation reaction 5h~12h；
Step 3: being cooled to 15 DEG C~40 DEG C, and neutralizer is added and adjusts pH value to 6~7 to get the single-component water-based organosilicon
Paper mould release.
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| CN111691218A (en) * | 2020-05-22 | 2020-09-22 | 仙鹤股份有限公司 | Preparation method of high-performance release paper |
| CN113024810A (en) * | 2021-03-23 | 2021-06-25 | 南昌大学 | Single-component self-crosslinkable fluorosilicone release agent and preparation method thereof |
| CN115368569A (en) * | 2022-09-06 | 2022-11-22 | 万华化学集团股份有限公司 | Branched polysiloxane and preparation method and application thereof |
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