CN109439170A - A kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable- - Google Patents
A kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable- Download PDFInfo
- Publication number
- CN109439170A CN109439170A CN201811415193.1A CN201811415193A CN109439170A CN 109439170 A CN109439170 A CN 109439170A CN 201811415193 A CN201811415193 A CN 201811415193A CN 109439170 A CN109439170 A CN 109439170A
- Authority
- CN
- China
- Prior art keywords
- parts
- added
- artificial leather
- modified
- fire
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
-
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- 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
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Synthetic Leather, Interior Materials Or Flexible Sheet Materials (AREA)
- Treatment And Processing Of Natural Fur Or Leather (AREA)
Abstract
The invention discloses a kind of artificial leather surface dulling-fire-retardant processing methods of anti-skid wearable-, and modified nano calcium carbonate and modified manometer silicon dioxide are added in aqueous polyurethane, heat magnetic agitation, plasticizer glycerol is added, continue to stir, stand degassing, non-skid coating is made；Gained non-skid coating and styrene methyl methacrylate lotion are mixed, emulsifier op-10 is added, stirs and blending emulsion is made；Blending emulsion is placed in dispersion machine, DOPO derivative flame retardant, levelling agent, crosslinking agent and gained surface cladding-modification by coupling modified titanium is added, it is fully dispersed uniform, the slurry made bar spreader is scratched on the surface of artificial leather, it spontaneously dries, obtains surface dulling-anti-skid wearable-flame retardant treatment artificial leather.
Description
Technical field
The invention belongs to artificial leather fields, and in particular to a kind of artificial leather surface dulling-fire-retardant processing side of anti-skid wearable-
Method.
Background technique
Currently, the surface dulling of artificial leather generallys use solvent type surface treating agent, wherein containing 85 ~ 90%
Organic solvent, a large amount of organic solvent can with drying be discharged into environment, serious pollution is caused to environment,
And the residual of solvent is so that final products have unpleasant solvent odor, and further endanger the health of consumer.With
The reinforcement of environmental regulation and people's environmental consciousness, using aqueous polyurethane as the environment-friendly type artificial leather surface treating agent of film forming matter at
For the research hotspot in the field.But single aqueous polyurethane not only levelability is bad on artificial leather surface, bonding force not
Foot, surface color wet rubbing are unqualified, and are difficult to reach the extinction effect of depth.
Summary of the invention
The purpose of the present invention is being directed to existing problem, it is fire-retardant to provide a kind of artificial leather surface dulling-anti-skid wearable-
Processing method, the artificial leather according to this method preparation have excellent anti-skid wearable performance and flame retardant property.
The present invention is achieved by the following technical solutions:
A kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable-, which comprises the steps of:
(1) the surface cladding of titanium dioxide-modification by coupling is modified:
5-6 parts of fine titanium dioxides and 0.9-1 parts of butyl titanates are distributed in 30-32 parts of dehydrated alcohols, magnetic agitation 60-
70min obtains A liquid；By in 7-8 parts of anhydrous liquor-saturated 0.5-1 parts of deionized waters of addition of second, stirring 30-40min obtains B liquid；Under strong stirring,
B drop is added in A liquid, continues after stirring 1-2h, is aged 24-25h, the titanium dioxide magnetic force for being aged rear surface coating modification is stirred
It mixes 20-30min to be uniformly dispersed, 0.2-0.3 parts of compounding coupling agents is added, continue to stir 20-30min, it is cold in 80-85 DEG C of oil bath
After solidifying back flow reaction 3-4h, precipitating is washed with water, alcohol is washed 3-5 times, is dried 20-24h in 80-85 DEG C of vacuum drying oven, is ground up, sieved,
Obtain surface cladding-modification by coupling modified titanium；
(2) modified Nano particle prepares non-skid coating:
Modified nano calcium carbonate and modified manometer silicon dioxide are added in 85-100 parts of aqueous polyurethanes, at 80-85 DEG C
Magnetic agitation 5-10min is heated, 2-3 parts of plasticizer glycerol are added, continues to stir 60-70min, stands degassing 20-30min, system
Obtain non-skid coating；
(3) artificial leather surface dulling-fire-retardant processing method of anti-skid wearable-:
Gained non-skid coating in (2) and 15-18 parts of styrene methyl methacrylate lotions are mixed, 1-2 parts of emulsifiers are added
OP-10 stirs 1-2h at 50-55 DEG C, and blending emulsion is made；Blending emulsion is placed in dispersion machine, DOPO derivative is added
Fire retardant, 0.01-0.02 part levelling agent, 1-2 parts of crosslinking agents and (1) middle gained surface cladding-modification by coupling modified titanium, fill
It is uniformly dispersed, the slurry made bar spreader is scratched on the surface of artificial leather, spontaneously dries, obtains surface dulling-
Anti-skid wearable-flame retardant treatment artificial leather.
Further, in step (1) titanium dioxide mechanical treatment process: titanium dioxide and dehydrated alcohol 1:1 are added to grinder
It after middle milled processed 20-40min, filtered, dried, is finely ground, obtaining fine titanium dioxide.
Further, compounding coupling agent is massaged by alkanolamine titanate coupling agent and silane coupling agent KH560 in step (1)
You form than 1:1.
Further, the surface of nanometer calcium carbonate is modified in step (2): into 6-8 parts of nanometer calcium carbonates, 1:10 addition is gone
At 60-65 DEG C after agitating and heating 50-60min, 0.18-0.24 parts of modifying agent odium stearate are added in ionized water, and ultrasonic vibration fills
Divide reaction 3-4h, with washes of absolute alcohol 3-5 times, centrifugation, dry 4-5h, grinds to obtain modified Nano carbon in 60-65 DEG C of baking oven
Sour calcium.
Further, the surface of nano silica is modified in step (2): into 1-2 parts of nano silicas, 1:10 adds
Enter dehydrated alcohol, stirs；0.2-0.4 parts of silane coupling agent KH570 are added to absolute ethanol, adjusting pH value with glacial acetic acid is 3-
4, stirring is lower to be mixed with the ethanol solution of nano silica, and heating stirring sufficiently reacts 4-5h at 80-85 DEG C, vacuum
It filters, the dry 4-5h in 60-65 DEG C of baking oven, grinds to obtain modified manometer silicon dioxide.
Further, in step (3) DOPO derivative flame retardant preparation: into 8-9 parts of glycidyl diethanolamines
15-16 parts of dehydrated alcohols are added, are warming up to 115-125 DEG C, is added with stirring 10-11 parts of DOPO reaction 7-8h, distilled water is added
Precipitating, is filtered to remove filtrate, precipitating is repeatedly washed with distilled water, be dried in vacuo 10-12h at 80-85 DEG C, and it is derivative to obtain DOPO
Object fire retardant.
The present invention has the advantage that compared with prior art
(1) amorphous titania cladding first is carried out to titanium dioxide, then organically-modified with coupling agent progress is compounded, obtains surface packet
- modification by coupling modified titanium is covered, can be used as nano modification delustering agent；By inorganic coating to titanium dioxide and organically-modified,
Improve powder using the space steric effect of the more organo-functional group in titanium dioxide surface
The reunion situation of body, it is 120 °, after surface-modified that contact angle, which significantly increases, after compounding is coupling agent modified, and compounding is even
Connection agent and surfactant can successfully be grafted to powder surface, and coupling agent group is present in powder surface, and powder surface is by parent
Aqueous to become lipophilic, contact angle increases.
(2) made with nanometer calcium carbonate and nano silica for anti-skidding pellet with odium stearate and silane coupling agent KH570
For modifying agent, processing is modified to nanometer calcium carbonate and nano silica respectively；With aqueous polyurethane for anti-skidding resin, with
Glycerol is plasticizer, prepares non-skid coating using blending method is dissolved；The grafting rate and oil-wetness of modified nanoparticle obtain
Preferably, the two compounding may make artificial leather to have preferable skid resistance and resistance to dispersibility to raising, and in aqueous polyurethane
Mill property.
(3) DOPO derivative flame retardant is compounded with modified manometer silicon dioxide, is used to prepare flame retardant artificial leather, it can be made
With excellent mechanical performance and smoke suppressing；Using the method for blending and modifying, styrene methyl methacrylate cream is utilized
Liquid is modified aqueous polyurethane, using blending emulsion as film forming matter, is prepared for environment-friendly type artificial leather surface dulling inorganic agent,
The emulsion particle of styrene methyl methacrylate and aqueous polyurethane can form core-shell structure, improve two kinds of lotions
Compatibility, film forming have certain extinction effect, show better mechanical property and water resistance；Styrene-methyl propylene
Contain a large amount of polar group on sour methyl esters and aqueous polyurethane strand, hydrogen bond can be formed between strand, it can also be with
The polar group on artificial leather surface forms Hydrogenbond, effectively increases blending emulsion film forming in the bonding energy on artificial leather surface
Power, the good combination property of film forming.
Specific embodiment
Embodiment 1
A kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable-, which comprises the steps of:
(1) the surface cladding of titanium dioxide-modification by coupling is modified:
5 parts of fine titanium dioxides and 0.9 part of butyl titanate are distributed in 30 parts of dehydrated alcohols, magnetic agitation 60min obtains A liquid；
By in 7 parts of anhydrous liquor-saturated additions of second, 0.5 part of deionized water, stirring 30min obtains B liquid；Under strong stirring, B drop is added in A liquid,
Continue after stirring 1h, for 24 hours, the titanium dioxide magnetic agitation 20min for being aged rear surface coating modification is uniformly dispersed for ageing, is added
0.2 part of compounding coupling agent, continues to stir 20min, and after reaction 3h is condensed back in 80-85 DEG C of oil bath, precipitating is washed with water, alcohol is washed
3 times, 20h is dried in 80-85 DEG C of vacuum drying oven, is ground up, sieved, obtains surface cladding-modification by coupling modified titanium；
(2) modified Nano particle prepares non-skid coating:
Modified nano calcium carbonate and modified manometer silicon dioxide are added in 85 parts of aqueous polyurethanes, heated at 80-85 DEG C
2 parts of plasticizer glycerol are added in magnetic agitation 5min, continue to stir 60min, stand degassing 20min, non-skid coating is made；
(3) artificial leather surface dulling-fire-retardant processing method of anti-skid wearable-:
Gained non-skid coating in (2) and 15 parts of styrene methyl methacrylate lotions are mixed, 1 part of polyoxyethylene nonylphenol ether-is added
10,1h is stirred at 50-55 DEG C, blending emulsion is made；Blending emulsion is placed in dispersion machine, it is fire-retardant that DOPO derivative is added
Agent, 0.01 part of levelling agent, 1 part of crosslinking agent and (1) middle gained surface cladding-modification by coupling modified titanium, it is fully dispersed uniform,
The slurry made bar spreader is scratched on the surface of artificial leather, spontaneously dries, obtains surface dulling-anti-skid wearable-resistance
Fire the artificial leather of processing.
Further, in step (1) titanium dioxide mechanical treatment process: titanium dioxide and dehydrated alcohol 1:1 are added to grinder
It after middle milled processed 20min, filtered, dried, is finely ground, obtaining fine titanium dioxide.
Further, compounding coupling agent is massaged by alkanolamine titanate coupling agent and silane coupling agent KH560 in step (1)
You form than 1:1.
Further, the surface of nanometer calcium carbonate is modified in step (2): into 6 parts of nanometer calcium carbonates 1:10 addition go from
At 60-65 DEG C after agitating and heating 50min, 0.18 part of modifying agent odium stearate is added in sub- water, and ultrasonic vibration sufficiently reacts 3h,
With washes of absolute alcohol 3 times, centrifugation, dry 4h, grinds to obtain modified nano calcium carbonate in 60-65 DEG C of baking oven.
Further, the surface of nano silica is modified in step (2): into 1 part of nano silica, 1:10 is added
Dehydrated alcohol, stirring；0.2 part of silane coupling agent KH570 is added to absolute ethanol, adjusting pH value with glacial acetic acid is 3-4, stirring
Lower to mix with the ethanol solution of nano silica, heating stirring sufficiently reacts 4h at 80-85 DEG C, be filtered by vacuum,
Dry 4h, grinds to obtain modified manometer silicon dioxide in 60-65 DEG C of baking oven.
Further, in step (3) DOPO derivative flame retardant preparation: into 8 parts of glycidyl diethanolamines plus
Enter 15 parts of dehydrated alcohols, be warming up to 115-125 DEG C, is added with stirring 10 parts of DOPO reaction 7h, distillation water sedimentation, filtering is added
Filtrate is removed, precipitating is repeatedly washed with distilled water, is dried in vacuo 10h at 80-85 DEG C, obtains DOPO derivative flame retardant.
Embodiment 2
A kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable-, which comprises the steps of:
(1) the surface cladding of titanium dioxide-modification by coupling is modified:
6 parts of fine titanium dioxides and 1 part of butyl titanate are distributed in 32 parts of dehydrated alcohols, magnetic agitation 70min obtains A liquid；By 8
In part 1 part of deionized water of the anhydrous liquor-saturated addition of second, stirring 40min obtains B liquid；Under strong stirring, B drop is added in A liquid, continues to stir
After mixing 2h, it is aged 25h, the titanium dioxide magnetic agitation 30min for being aged rear surface coating modification is uniformly dispersed, is added 0.3 part again
With coupling agent, continue to stir 30min, after reaction 4h is condensed back in 80-85 DEG C of oil bath, precipitating is washed with water, alcohol is washed 5 times,
It dries for 24 hours, is ground up, sieved in 80-85 DEG C of vacuum drying oven, obtain surface cladding-modification by coupling modified titanium；
(2) modified Nano particle prepares non-skid coating:
Modified nano calcium carbonate and modified manometer silicon dioxide are added in 100 parts of aqueous polyurethanes, heated at 80-85 DEG C
3 parts of plasticizer glycerol are added in magnetic agitation 10min, continue to stir 70min, stand degassing 30min, non-skid coating is made；
(3) artificial leather surface dulling-fire-retardant processing method of anti-skid wearable-:
Gained non-skid coating in (2) and 18 parts of styrene methyl methacrylate lotions are mixed, 2 parts of polyoxyethylene nonylphenol ethers-are added
10,2h is stirred at 50-55 DEG C, blending emulsion is made；Blending emulsion is placed in dispersion machine, it is fire-retardant that DOPO derivative is added
Agent, 0.02 part of levelling agent, 2 parts of crosslinking agents and (1) middle gained surface cladding-modification by coupling modified titanium, it is fully dispersed uniform,
The slurry made bar spreader is scratched on the surface of artificial leather, spontaneously dries, obtains surface dulling-anti-skid wearable-resistance
Fire the artificial leather of processing.
Further, in step (1) titanium dioxide mechanical treatment process: titanium dioxide and dehydrated alcohol 1:1 are added to grinder
It after middle milled processed 40min, filtered, dried, is finely ground, obtaining fine titanium dioxide.
Further, compounding coupling agent is massaged by alkanolamine titanate coupling agent and silane coupling agent KH560 in step (1)
You form than 1:1.
Further, the surface of nanometer calcium carbonate is modified in step (2): into 8 parts of nanometer calcium carbonates 1:10 addition go from
At 60-65 DEG C after agitating and heating 60min, 0.24 part of modifying agent odium stearate is added in sub- water, and ultrasonic vibration sufficiently reacts 4h,
With washes of absolute alcohol 5 times, centrifugation, dry 5h, grinds to obtain modified nano calcium carbonate in 60-65 DEG C of baking oven.
Further, the surface of nano silica is modified in step (2): into 2 parts of nano silicas, 1:10 is added
Dehydrated alcohol, stirring；0.4 part of silane coupling agent KH570 is added to absolute ethanol, adjusting pH value with glacial acetic acid is 3-4, stirring
Lower to mix with the ethanol solution of nano silica, heating stirring sufficiently reacts 5h at 80-85 DEG C, be filtered by vacuum,
Dry 5h, grinds to obtain modified manometer silicon dioxide in 60-65 DEG C of baking oven.
Further, in step (3) DOPO derivative flame retardant preparation: into 9 parts of glycidyl diethanolamines plus
Enter 16 parts of dehydrated alcohols, be warming up to 115-125 DEG C, is added with stirring 11 parts of DOPO reaction 8h, distillation water sedimentation, filtering is added
Filtrate is removed, precipitating is repeatedly washed with distilled water, is dried in vacuo 12h at 80-85 DEG C, obtains DOPO derivative flame retardant.
Comparative example 1
This comparative example 1 compared with Example 1, does not appoint nanometer calcium carbonate and nano silica in step (2)
What modification, method and step in addition to this are all the same.
Comparative example 2
This comparative example 2 compared with Example 2, does not prepare DOPO derivative flame retardant in step (3), but directly adds
DOPO, method and step in addition to this are all the same.
The pure artificial leather of control group
It is real to above-described embodiment 1, embodiment 2, comparative example 1, comparison in order to compare the performance of artificial leather produced by the present invention
It applies the corresponding artificial leather obtained of 2 method of example and the corresponding pure artificial leather of control group and carries out performance detection, tool according to professional standard
Body correlation data is as shown in table 1 below:
Table 1
| Project | Coefficient of friction | Total smoke-producing amount | Tensile strength |
| Embodiment 1 | 0.64 | Reduce 26% | Improve 32% |
| Embodiment 2 | 0.62 | Reduce 27% | Improve 33% |
| Comparative example 1 | 0.81 | Reduce 25% | Improve 31% |
| Comparative example 2 | 0.63 | Reduce 10% | Improve 12% |
| Control group | 0.92 | / | / |
There is excellent anti-skid wearable performance and flame retardant property according to the artificial leather of the method for the present invention preparation, according to the method for the present invention
Glossiness < 10% of the artificial leather system of processing, can satisfy the requirement of deep dull product；The dry and wet of artificial leather surface color
Rubbing fastness > 4 grade have reached national standard.
Any modification is not carried out to nanometer calcium carbonate and nano silica in comparative example 1, is caused artificial
The coefficient of friction of leather increases, but compares and appoint so with preferable skid resistance and wearability with pure artificial leather；In comparative example 2
DOPO derivative flame retardant is not prepared but directly adds DOPO, causes the flame retarding and smoke suppressing properties of artificial leather and mechanical performance equal
It reduces, but compare with pure artificial leather flame retarding and smoke suppressing properties and mechanical performance times so increases.
Claims (6)
1. a kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable-, which comprises the steps of:
(1) the surface cladding of titanium dioxide-modification by coupling is modified:
5-6 parts of fine titanium dioxides and 0.9-1 parts of butyl titanates are distributed in 30-32 parts of dehydrated alcohols, magnetic agitation 60-
70min obtains A liquid；By in 7-8 parts of anhydrous liquor-saturated 0.5-1 parts of deionized waters of addition of second, stirring 30-40min obtains B liquid；Under strong stirring,
B drop is added in A liquid, continues after stirring 1-2h, is aged 24-25h, the titanium dioxide magnetic force for being aged rear surface coating modification is stirred
It mixes 20-30min to be uniformly dispersed, 0.2-0.3 parts of compounding coupling agents is added, continue to stir 20-30min, it is cold in 80-85 DEG C of oil bath
After solidifying back flow reaction 3-4h, precipitating is washed with water, alcohol is washed 3-5 times, is dried 20-24h in 80-85 DEG C of vacuum drying oven, is ground up, sieved,
Obtain surface cladding-modification by coupling modified titanium；
(2) modified Nano particle prepares non-skid coating:
Modified nano calcium carbonate and modified manometer silicon dioxide are added in 85-100 parts of aqueous polyurethanes, at 80-85 DEG C
Magnetic agitation 5-10min is heated, 2-3 parts of plasticizer glycerol are added, continues to stir 60-70min, stands degassing 20-30min, system
Obtain non-skid coating；
(3) artificial leather surface dulling-fire-retardant processing method of anti-skid wearable-:
Gained non-skid coating in (2) and 15-18 parts of styrene methyl methacrylate lotions are mixed, 1-2 parts of emulsifiers are added
OP-10 stirs 1-2h at 50-55 DEG C, and blending emulsion is made；Blending emulsion is placed in dispersion machine, DOPO derivative is added
Fire retardant, 0.01-0.02 part levelling agent, 1-2 parts of crosslinking agents and (1) middle gained surface cladding-modification by coupling modified titanium, fill
It is uniformly dispersed, the slurry made bar spreader is scratched on the surface of artificial leather, spontaneously dries, obtains surface dulling-
Anti-skid wearable-flame retardant treatment artificial leather.
2. a kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable-according to claim 1, feature exist
In titanium dioxide and dehydrated alcohol 1:1 the mechanical treatment process of titanium dioxide in step (1): are added to milled processed 20- in grinder
It after 40min, filtered, dried, is finely ground, obtaining fine titanium dioxide.
3. a kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable-according to claim 1, feature exist
In by alkanolamine titanate coupling agent and silane coupling agent KH560,1:1 is formed compounding coupling agent in molar ratio in step (1).
4. a kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable-according to claim 1, feature exist
In the surface of nanometer calcium carbonate is modified in step (2): into 6-8 parts of nanometer calcium carbonates, deionized water is added in 1:10, in 60-65
At DEG C after agitating and heating 50-60min, 0.18-0.24 parts of modifying agent odium stearate are added, ultrasonic vibration sufficiently reacts 3-4h, uses
Washes of absolute alcohol 3-5 times, centrifugation, dry 4-5h, grinds to obtain modified nano calcium carbonate in 60-65 DEG C of baking oven.
5. a kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable-according to claim 1, feature exist
In the surface of nano silica is modified in step (2): into 1-2 parts of nano silicas, dehydrated alcohol is added in 1:10, is stirred
It mixes；0.2-0.4 parts of silane coupling agent KH570 are added to absolute ethanol, adjusting pH value with glacial acetic acid is 3-4, and stirring is descended and received
The ethanol solution mixing of rice silica, heating stirring sufficiently reacts 4-5h at 80-85 DEG C, is filtered by vacuum, in 60-65
Dry 4-5h, grinds to obtain modified manometer silicon dioxide in DEG C baking oven.
6. a kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable-according to claim 1, feature exist
In the preparation of DOPO derivative flame retardant in step (3): into 8-9 parts of glycidyl diethanolamines, 15-16 parts of addition is anhydrous
Ethyl alcohol is warming up to 115-125 DEG C, is added with stirring 10-11 parts of DOPO reaction 7-8h, distillation water sedimentation is added, is filtered to remove filter
Liquid repeatedly washs precipitating with distilled water, is dried in vacuo 10-12h at 80-85 DEG C, obtains DOPO derivative flame retardant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811415193.1A CN109439170A (en) | 2018-11-26 | 2018-11-26 | A kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable- |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811415193.1A CN109439170A (en) | 2018-11-26 | 2018-11-26 | A kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable- |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109439170A true CN109439170A (en) | 2019-03-08 |
Family
ID=65555414
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811415193.1A Pending CN109439170A (en) | 2018-11-26 | 2018-11-26 | A kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable- |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109439170A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112175417A (en) * | 2020-09-26 | 2021-01-05 | 许荣 | Novel nanoscale liquid titanium dioxide for coating |
| CN112680085A (en) * | 2021-01-20 | 2021-04-20 | 浙江麦斯特姆涂布有限公司 | High-gloss scratch-resistant surface-enhanced artificial leather and preparation method thereof |
| CN113174777A (en) * | 2021-03-31 | 2021-07-27 | 美盈森集团股份有限公司 | Bi-component coating type anti-slip coating and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102533079A (en) * | 2011-12-08 | 2012-07-04 | 浙江深蓝轻纺科技有限公司 | Extinction-type water-based polyurethane finishing agent used for synthetic leather |
| CN103113712A (en) * | 2013-02-04 | 2013-05-22 | 佛山市科富科技有限公司 | Preparation method and application of modified nano-silicon dioxide toughened epoxy resin |
| WO2015107933A1 (en) * | 2014-01-15 | 2015-07-23 | Dic株式会社 | Aqueous surface treatment agent and product using same |
-
2018
- 2018-11-26 CN CN201811415193.1A patent/CN109439170A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102533079A (en) * | 2011-12-08 | 2012-07-04 | 浙江深蓝轻纺科技有限公司 | Extinction-type water-based polyurethane finishing agent used for synthetic leather |
| CN103113712A (en) * | 2013-02-04 | 2013-05-22 | 佛山市科富科技有限公司 | Preparation method and application of modified nano-silicon dioxide toughened epoxy resin |
| WO2015107933A1 (en) * | 2014-01-15 | 2015-07-23 | Dic株式会社 | Aqueous surface treatment agent and product using same |
Non-Patent Citations (6)
| Title |
|---|
| 李子东: "《实用胶粘剂原材料手册》", 31 July 1997, 国防工业出版业 * |
| 李毅辉: "DOPO衍生物阻燃剂的制备及在聚氨酯革上的应用", 《中国优秀硕士论文全文数据库》 * |
| 白涛: "《攀登者的足迹 百步梯攀登计划优秀论文汇编 2003》", 30 December 2004, 华南理工大学出版社 * |
| 童忠良: "《新型功能复合涂料与应用》", 30 September 2007, 国防工业出版社 * |
| 郑永林等: "《粉体表面改性 第3版》", 30 September 2011, 中国建材工业出版社 * |
| 郑永林等: "《非金属矿加工技术与应用手册》", 31 May 2005, 冶金工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112175417A (en) * | 2020-09-26 | 2021-01-05 | 许荣 | Novel nanoscale liquid titanium dioxide for coating |
| CN112680085A (en) * | 2021-01-20 | 2021-04-20 | 浙江麦斯特姆涂布有限公司 | High-gloss scratch-resistant surface-enhanced artificial leather and preparation method thereof |
| CN113174777A (en) * | 2021-03-31 | 2021-07-27 | 美盈森集团股份有限公司 | Bi-component coating type anti-slip coating and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109439170A (en) | A kind of artificial leather surface dulling-fire-retardant processing method of anti-skid wearable- | |
| CN112175418B (en) | Modified white carbon black, preparation method thereof and masterbatch | |
| CN114286800B (en) | Hydrophobic white carbon black rubber reinforcing agent and preparation method and application thereof | |
| CN114286801B (en) | Hydrophobic high-dispersion white carbon black and preparation method and application thereof | |
| CN110643214B (en) | High-dispersity precipitated silica anti-settling agent for coating and preparation method thereof | |
| WO1997012843A1 (en) | Microporous high structure precipitated silicas and methods | |
| CN105330784A (en) | Method for preparing waterborne acrylic resin | |
| CN106916515A (en) | A kind of Functional Powder Coating and preparation method thereof | |
| CN104130531B (en) | For polyvinyl chloride composite cable material and the manufacture method thereof of power domain | |
| CN110294942A (en) | Cold mixing chromatic bituminous cement and preparation method thereof | |
| DE10056696A1 (en) | Preparation of filler-containing rubber powder used for vulcanizable rubber mixtures, comprises using a salt-containing silicic acid precipitate suspension as a filler | |
| CN102198942A (en) | Preparation method of silicon dioxide | |
| CN103554377A (en) | Preparation method for coating of nano-silica through miniemulsion polymerization | |
| CN105907206A (en) | Preparation method of high-hardness abrasion-resistant water-borne wood paint | |
| CN108314762A (en) | Polymer-doped Nano-meter SiO_22Oil suction gel resin and its preparation method and application | |
| CN106590052A (en) | Polydopamine polyethenoxy ether active agent modified shape-controllable nano calcium carbonate powder and preparation method thereof | |
| CN102190802A (en) | Preparation method of cross-linked polymer wax micropowder | |
| CN109897245A (en) | Preparation method of styrene butadiene rubber composition containing carbon nano tubes and used for tire tread | |
| CN109319793A (en) | A kind of preparation method of Gao Bibiao, high oil absorption white carbon black | |
| CN110628240B (en) | Water-soluble composite modified grinding aid, preparation method and application | |
| CN104031429B (en) | A kind of surface-modified nano titanium dioxide with antiageing effect and preparation method thereof | |
| CN109897249A (en) | Preparation method of carbon nanotube-filled rubber composition | |
| CN106189473B (en) | The preparation method of automobile metal paint silica dioxide delustring agent | |
| CN106220903A (en) | A kind of preparation method of graphene oxide/sodium alginate composite | |
| CN106398315A (en) | Shape-controllable nano calcium carbonate powder modified by grafted AOS (Alpha Olefin Sulfonate) polyoxyethylene ether treating agent and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190308 |
|
| RJ01 | Rejection of invention patent application after publication |