CN109294076A - A kind of preparation method of halogen-free flameproof dynamic perduren waterproof roll - Google Patents
A kind of preparation method of halogen-free flameproof dynamic perduren waterproof roll Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/16—Elastomeric ethene-propene or ethene-propene-diene copolymers, e.g. EPR and EPDM rubbers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- 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
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- 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
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
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Abstract
The invention discloses a kind of preparation methods of halogen-free flameproof dynamic perduren waterproof roll, by using two double screw extruder linkages and each parameter of strict control double screw extruder, keep the production technology shear ability of dynamic perduren waterproof roll strong, it is each to be mutually kneaded uniformly, it is capable of forming uniform " island structure ", and rational allocation is carried out to each component dosage, products obtained therefrom physicochemical property is more excellent, stable product quality is good, and it can be realized continuous production, realize product quality real time monitoring, production technology production efficiency greatly improves, it can be with real-time online adjusting process, formula, reduce rejection rate.
Description
Technical field
The present invention relates to waterproof roll fields, in particular it relates to a kind of halogen-free flameproof dynamic perduren waterproof
The preparation method of coiled material.
Background technique
As construction industry flourishes, demand of the building engineering field to waterproof roll is also increasing, equally, to material
Quality requirements are also improving, thus provide wide space for the popularization and application of novel high polymer coiled material, at present domestic contrast
Mature macromolecule coiled material mainly has ethylene propylene diene rubber (EPDM) to vulcanize coiled material and polyvinyl chloride (PVC) waterproof roll etc..It is poly-
Vinyl chloride waterproof roll can accomplish continuous production, but coiled material is not ageing-resistant, and durability is poor, while polyvinyl chloride waterproof roll
It is commonly incorporated into O-phthalic acids plasticizer in material production, is caused damages to human body and environment, environmental-protecting performance is poor.Ethylene-propylene-diene monomer
Glue waterproofing membrane production complex process was needed by stages such as mixing, mill, filter glue, extrusion, vulcanizations, ripe to the operation of worker
Practicing degree and mechanical equipment has higher requirement.
Thermoplastic dynamic perduren (Thermoplastic Dynamic Vulcanizate), referred to as TPV are " dynamic
2 word of state " specifically illustrates the technique-dynamic vulcanization for producing this thermoplastic vulcanizates, and this technique refers in rubber and thermoplastic
Make the vulcanization of rubber in property plastic molten melt Blending Processes, also constantly mixed with thermoplastic certainly while the vulcanization of rubber,
Therefore the rubber that has cured be as dispersed phase distribution in thermoplastic continuous phase.Dynamic vulcanization technology uses advanced life
Production. art is different from prior art, the presence for having partial vulcanization or vulcanizing entirely, has fully ensured that the ageing-resistant performance of material, and
Production is environmentally friendly, pollution-free.But since waterproofing membrane production breadth is big, formula system is complicated, and product quality and mixing degree have directly
Relationship is connect, therefore controlling of production process is particularly important.
The Technology of Dynamic Vulcanized of the prior art mostly use greatly single single screw extrusion machine, double screw extruder, mixer with
The mode that single screw extrusion machine or mixer link with double screw extruder produces.Single extrusion machine operation melting effect is poor, modeling
Material cannot mutually form uniform " island structure " with rubber phase, keep product stability poor；Mixer and extruder linkage are certain
Mixing is solved the problems, such as in degree, but technique is more difficult to control, be unable to continuous production, real time monitoring ability is poor, and existing rubber
The most of flame retardant effects of glue are bad.Therefore it provides a kind of anti-flammability dynamic perduren waterproof roll for capableing of continuous production
Preparation method, make that the waterproof roll stability of preparation is strong, stable product quality, be of great significance.
Summary of the invention
Based on this, the invention reside in overcoming the deficiencies of existing technologies, a kind of halogen-free flameproof dynamic perduren waterproof is provided
The preparation method of coiled material, the waterproof roll excellent in mechanical performance prepared using the preparation method, acid and alkali-resistance, ageing-resistant performance
Good, excellent fireproof performance, quality stability is good, and being capable of continuous production.
Its technical solution is as follows:
A kind of preparation method of dynamic perduren waterproof roll, includes the following steps:
(1) by rubber, thermoplastic resin, cosolvent, reinforcing agent, softening agent, the catalysis for accounting for catalyst total amount 10%-25%
The first double screw extruder is added in agent, glidant, interface modifier, antioxidant, titanium dioxide, through plasticizing, shearing, mixing, extrusion
It obtains being kneaded item at a pelletizing, at 170-210 DEG C, the control of net-changing device temperature exists the first double screw extruder extruder barrel temperature control
190-220 DEG C, connection temperature control 190-220 DEG C, flange temperature control 190-220 DEG C, metering pump temperature control exist
190-220 DEG C, mold temperature control at 190-220 DEG C, metering pump speed 5.0-12.0rad/min, screw speed 100-190r/
min；
(2) item will be kneaded to be added in the second double screw extruder, and is proportionally added into crosslinking agent, cross-linking aid, residue
Catalyst, fire retardant dynamic vulcanization reaction completed, and squeeze out semi-finished product sheet material by melting, mixing, exhaust, metering, second
Double screw extruder extruder barrel temperature control is at 190-250 DEG C, and the control of net-changing device temperature is in 200-260 DEG C, connection temperature control
Exist in 200-260 DEG C, the control of metering pump temperature in 200-260 DEG C, mold temperature control in 200-260 DEG C, the control of flange temperature
200-260 DEG C, metering pump speed 5.0-12.0rad/min, screw speed 100-200r/min；
(3) it by the semi-finished product sheet material squeezed out through the second double screw extruder by calendering sizing, is most made afterwards through cooling, deposit
It is standby to obtain dynamic perduren waterproof roll finished product；
Wherein, each material is specific as follows: 20-30 parts of rubber；20-25 parts of thermoplastic resin；2-5 parts of cosolvent；Reinforcing agent
5-10 parts；5-10 parts of softening agent；5-10 parts of halogen-free flame retardants；0.3-1 parts of crosslinking agent；1-3 parts of cross-linking aid；Catalyst 2-3.5
Part；1-3 parts of glidant；1-3 parts of interface modifier；1-3 parts of antioxidant；5-10 parts of titanium dioxide.
The present invention makes by using two double screw extruder linkages and each parameter of strict control double screw extruder
The production technology shear ability of state vulcanized rubber waterproof roll is strong, each to be mutually kneaded uniformly, is capable of forming uniform " island structure ",
And rational allocation is carried out to each component dosage, products obtained therefrom physicochemical property is more excellent, and stable product quality is good；Nothing is added in system
Halogen fire retardant, and squeeze out and process through the second screw extruder, it is distributed to halogen-free flame retardants sufficiently uniformly in rubbery system, hinders
Combustion is had excellent performance, good environmental protection.Preparation method of the present invention realizes continuous production, realizes that product quality is supervised in real time
Control, production technology production efficiency greatly improve, and can reduce rejection rate with real-time online adjusting process, formula.
The first double screw extruder barrel temperature is segmented into 1 area's temperature of barrel temperature in one of the embodiments,
For 170-180 DEG C, 2 area's temperature be 175-185 DEG C, 3 area's temperature are 180-190 DEG C, 4 area's temperature are 180-195 DEG C, 5 area's temperature
For 185-200 DEG C, 6 area's temperature be 190-195 DEG C, 7 area's temperature are 185-195 DEG C, 8 area's temperature are 190-200 DEG C, 9 area's temperature
For 200-210 DEG C, 10 area's temperature be 210 DEG C.
The second double screw extruder barrel temperature is segmented into 1 area's temperature of barrel temperature in one of the embodiments,
For 190-200 DEG C, 2 area's temperature be 195-205 DEG C, 3 area's temperature are 200-215 DEG C, 4 area's temperature are 205-220 DEG C, 5 area's temperature
For 200-215 DEG C, 6 area's temperature be 195-215 DEG C, 7 area's temperature are 200-220 DEG C, 8 area's temperature are 200-225 DEG C, 9 area's temperature
For 230-250 DEG C, 10 area's temperature be 230-250 DEG C.
The rubber is ethylene propylene diene rubber and/or butyl rubber, wherein ethylene-propylene-diene monomer in one of the embodiments,
The ethylene contents of glue are 55%-75%.
The halogen-free flame retardants is the mixture of phosphorus flame retardant and inorganic fire retardants in one of the embodiments,.
The halogen-free flame retardants is the phosphorus flame retardant handled by surfactant and nothing in one of the embodiments,
The mixture of machine fire retardant.Surfactant processing can increase the compatibility of halogen-free flame retardants Yu other components of rubbery system,
The especially compatibility of inorganic fire retardants and rubber makes halogen-free flame retardants dispersion more evenly, and flame retardant effect is more preferable.
The cosolvent is maleic anhydride, glycidyl methacrylate, metering system in one of the embodiments,
Sour hydroxyl ethyl ester grafted polyethylene, polypropylene or polyolefin elastomer.
The reinforcing agent is coumarone indene resin, Petropols, phenolic resin, rosin resin in one of the embodiments,
One of or it is a variety of.
The softening agent is naphthenic oil and/or paraffin oil in one of the embodiments,.
The crosslinking agent is cumyl peroxide, in two isobutylbenzene of peroxidating, sulphur in one of the embodiments,
It is one or more.
The cross-linking aid is three acrylic isocyanuric acid esters, trimethylolpropane tris first in one of the embodiments,
One of base acrylate, promotor PZ or a variety of.
In one of the embodiments, the catalyst be nano zine oxide, stearic acid, Co, Ni it is one or more.
In one of the embodiments, the glidant be chlorinated paraffin, oxidized polyethylene wax, one kind of calcium stearate or
It is a variety of.Glidant is capable of providing good processing fluidity, reduces the frictional property with screw extruder, prevents bonding with screw rod
Caused by aging.
The interface modifier is that silane coupling agent, aluminate coupling agent or titanate esters are even in one of the embodiments,
Join one of agent or a variety of.
The antioxidant was four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] seasons in one of the embodiments,
Doutrate, β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid n-octadecyl alcohol ester,；Three (2,4- di-tert-butyl-phenyls) are sub-
Phosphoric acid it is one or more.
The titanium dioxide is rutile type titanium white in one of the embodiments,.Rutile type titanium white have reinforcement,
Anti-aging, filling effect, stability of crystal form is good, improves the color and photostability of dynamic perduren waterproof roll.
The beneficial effects of the present invention are: (1) present invention using two double screw extruder linkages squeeze out preparation dynamic sulphur
Change rubber water-proofing coiled, realizes continuous production, product quality can monitor in real time；(2) dynamic vulcanization rubber of the present invention
The production technology shear ability of glue waterproof roll is strong, each to be mutually kneaded uniformly, is capable of forming uniform " island structure ", and product is physical and chemical
Performance is more excellent, stable product quality；(3) halogen-free flame retardants is added in system, and squeezes out and processes through the second screw extruder, is made
Halogen-free flame retardants is sufficiently uniformly distributed in rubbery system, excellent fireproof performance, good environmental protection；(4) dynamic of the invention
The production technology production efficiency of vulcanized rubber waterproof roll greatly improves, and real-time online adjusting process, formula reduce rejection rate.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention more comprehensible, below in conjunction with specific embodiment, to this
Invention is described in further detail.It should be understood that the specific embodiments described herein are only to explain this hair
It is bright, and the scope of protection of the present invention is not limited.
Raw materials used following embodiment is ordinary commercial products.
Halogen-free flame retardants used in following embodiment is prepared as follows to obtain:
1 part of pentaerythrite, 0.5 part of aluminate coupling agent, 5.8 parts of melamine phosphates, 2.7 parts of aluminium hydroxides are mixed
It closes, stirs 30-60min at 60-70 DEG C up to the halogen-free flame retardants.
Embodiment 1
A kind of preparation method of dynamic perduren waterproof roll, includes the following steps:
(1) by 20 parts of ethylene propylene diene rubbers (EPDM), 20 parts of polyethylene (PE), 5 parts of maleic anhydride grafted polyethylene (MAH-
G-PE), 10 parts of coumarone indene resins, 5 parts of naphthenic oils (KN-4010), 0.5 part of Co, 1 part of oxidized polyethylene wax (OPE wax), 1 part of silicon
Alkane coupling agent (KH-550), 1 part of antioxidant 1010,1 part of irgasfos 168,5 parts of titanium dioxides pass through weightless title in proportion and are added first
Double screw extruder through plasticizing, shearing, is kneaded, is extruded into a pelletizing, and the first double screw extruder extruder barrel temperature control is in 170-
210 DEG C, net-changing device temperature control 210 DEG C, connection temperature control 210 DEG C, flange temperature control in 210 DEG C, metering pump
Temperature control is in 210 DEG C, mold temperature control at 215 DEG C, metering pump speed 7.0rad/min, screw speed 130-145r/
Min, to ensure that it is uniform that each component is kneaded；More specifically, the first double screw extruder barrel temperature is segmented into 1 area's temperature of barrel temperature
Degree is 170 DEG C, 2 area's temperature are 175 DEG C, 3 area's temperature are 180 DEG C, 4 area's temperature are 180 DEG C, 5 area's temperature are 185 DEG C, 6 area's temperature
For 190 DEG C, 7 area's temperature be 195 DEG C, 8 area's temperature are 200 DEG C, 9 area's temperature are 210 DEG C, 10 area's temperature are 210 DEG C.
(2) by the first twin-screw extrusion machining squeeze out mixing item be added in the second double screw extruder, and by than
0.3 part of cumyl peroxide (DCP), 1 part of three acrylic isocyanuric acid ester (TAIC), 0.5 part of nano zine oxide is added in example
(ZnO), 1 part of stearic acid (SA), 8 parts of halogen-free flame retardants complete dynamic vulcanization reaction by melting, mixing, exhaust, metering, and
Squeeze out semi-finished product sheet material, the second double screw extruder extruder barrel temperature control 190-230 DEG C, net-changing device temperature control 230 DEG C,
Temperature control is connected to control in 230 DEG C, the control of metering pump temperature in 230 DEG C, mold temperature in 230 DEG C, the control of flange temperature
At 230 DEG C, metering pump speed 8.0rad/min, screw speed 100r/min；More specifically, the second double screw extruder machine
Cylinder temperature section be 1 area's temperature of barrel temperature be 190 DEG C, 2 area's temperature are 195 DEG C, 3 area's temperature are 200 DEG C, 4 area's temperature are 205
DEG C, 5 area's temperature be 210 DEG C, 6 area's temperature are 215 DEG C, 7 area's temperature are 220 DEG C, 8 area's temperature are 225 DEG C, 9 area's temperature are 230
DEG C, 10 area's temperature be 230 DEG C.
(3) sheet material for squeezing out the second double screw extruder is by the sizing of three-roller calendaring system, most afterwards through cooling, Chu Bu,
Be prepared dynamic perduren waterproof roll finished product, the dynamic perduren waterproof roll of preparation with a thickness of 1mm, dynamic sulphur
Changing rubber water-proofing coiled width is 2000mm, and the length of dynamic perduren waterproof roll is 20m.
Embodiment 2
A kind of preparation method of dynamic perduren waterproof roll, includes the following steps:
(1) by 20 parts of ethylene propylene diene rubbers (EPDM), 25 parts of polyethylene (PE), 2 parts of maleic anhydride grafted polyethylene (MAH-
G-PE), 5 parts of coumarone indene resins, 5 parts of naphthenic oils (KN-4010), 0.5 part of Co, 1 part of oxidized polyethylene wax (OPE wax), 1 part of silane
Coupling agent (KH-550), 1 part of antioxidant 1010,1 part of irgasfos 168,5 parts of titanium dioxides pass through weightless title in proportion and are added first pair
Screw extruder through plasticizing, shearing, is kneaded, is extruded into a pelletizing, and the first double screw extruder extruder barrel temperature control is in 180-
210 DEG C, net-changing device temperature control 215 DEG C, connection temperature control 215 DEG C, flange temperature control in 215 DEG C, metering pump
Temperature control is in 215 DEG C, mold temperature control at 215 DEG C, metering pump speed 8.0rad/min, screw speed 140-160r/
Min, to ensure that it is uniform that each component is kneaded；More specifically, the first double screw extruder barrel temperature is segmented into 1 area's temperature of barrel temperature
Degree is 180 DEG C, 2 area's temperature are 185 DEG C, 3 area's temperature are 190 DEG C, 4 area's temperature are 190 DEG C, 5 area's temperature are 195 DEG C, 6 area's temperature
For 195 DEG C, 7 area's temperature be 195 DEG C, 8 area's temperature are 200 DEG C, 9 area's temperature are 210 DEG C, 10 area's temperature are 210 DEG C.
(2) by the first twin-screw extrusion machining squeeze out mixing item be added in the second double screw extruder, and by than
0.5 part of cumyl peroxide (DCP), 1 part of three acrylic isocyanuric acid ester (TAIC), 2 parts of nano zine oxides is added in example
(ZnO), 1 part of stearic acid (SA), 5 parts of halogen-free flame retardants complete dynamic vulcanization reaction by melting, mixing, exhaust, metering, and
Squeeze out semi-finished product sheet material, the second double screw extruder extruder barrel temperature control 200-230 DEG C, net-changing device temperature control 230 DEG C,
Temperature control is connected to control in 230 DEG C, the control of metering pump temperature in 230 DEG C, mold temperature in 230 DEG C, the control of flange temperature
At 235 DEG C, metering pump speed 10.0rad/min, screw speed 160r/min；More specifically, second double screw extruder
Barrel temperature is segmented into that 1 area's temperature of barrel temperature is 200 DEG C, 2 area's temperature are 205 DEG C, 3 area's temperature are 205 DEG C, 4 area's temperature are
210 DEG C, 5 area's temperature be 210 DEG C, 6 area's temperature are 215 DEG C, 7 area's temperature are 220 DEG C, 8 area's temperature are 225 DEG C, 9 area's temperature are
230 DEG C, 10 area's temperature be 230 DEG C.
(3) sheet material for squeezing out the second double screw extruder is by the sizing of double roller calendaring system, most afterwards through cooling, Chu Bu,
Be prepared dynamic perduren waterproof roll finished product, the dynamic perduren waterproof roll of preparation with a thickness of 0.8mm, dynamic
The width of vulcanized rubber waterproof roll is 2000mm, and the length of dynamic perduren waterproof roll is 20m.
Embodiment 3
A kind of preparation method of dynamic perduren waterproof roll, includes the following steps:
(1) by 30 parts of ethylene propylene diene rubbers (EPDM), 20 parts of polyethylene (PE), 10 parts of maleic anhydride grafted polyethylenes
(MAH-g-PE), 8 parts of coumarone indene resins, 10 parts of naphthenic oils (KN-4010), 1 part of Co, 3 parts of oxidized polyethylene wax (OPE wax), 3 parts
Silane coupling agent (KH-550), 1.5 parts of antioxidant 1010s, 1.5 parts of irgasfos 168s, 10 parts of titanium dioxides pass through weightless title in proportion
The first double screw extruder is added, through plasticizing, shearing, is kneaded, is extruded into a pelletizing, the first double screw extruder barrel temperature control
System is controlled in 210 DEG C, flange temperature 210 in 170-210 DEG C, the control of net-changing device temperature in 210 DEG C, the control of connection temperature
DEG C, the control of metering pump temperature in 210 DEG C, mold temperature control at 215 DEG C, metering pump speed 7.0rad/min, screw speed
155-175r/min, to ensure that it is uniform that each component is kneaded；More specifically, the first double screw extruder barrel temperature is segmented into machine barrel
1 area's temperature of temperature is 170 DEG C, 2 area's temperature are 175 DEG C, 3 area's temperature are 180 DEG C, 4 area's temperature are 180 DEG C, 5 area's temperature are 185
DEG C, 6 area's temperature be 190 DEG C, 7 area's temperature are 195 DEG C, 8 area's temperature are 200 DEG C, 9 area's temperature are 210 DEG C, 10 area's temperature are 210
℃。
(2) by the first twin-screw extrusion machining squeeze out mixing item be added in the second double screw extruder, and by than
1 part of cumyl peroxide (DCP), 3 part of three acrylic isocyanuric acid ester (TAIC), 1 part of nano zine oxide (ZnO), 1 is added in example
Part stearic acid (SA), 10 parts of halogen-free flame retardants complete dynamic vulcanization reaction by melting, mixing, exhaust, metering, and squeeze out half
Finished sheet, the second double screw extruder extruder barrel temperature control is in 190-230 DEG C, the control of net-changing device temperature in 230 DEG C, connector
Temperature control is controlled in 230 DEG C, mold temperature 230 in 230 DEG C, the control of flange temperature in 230 DEG C, the control of metering pump temperature
DEG C, metering pump speed 8.0rad/min, screw speed 200r/min；More specifically, the second double screw extruder machine barrel temperature
Degree is segmented into that 1 area's temperature of barrel temperature is 190 DEG C, 2 area's temperature are 195 DEG C, 3 area's temperature are 200 DEG C, 4 area's temperature are 205 DEG C, 5
Area's temperature is 210 DEG C, 6 area's temperature are 215 DEG C, 7 area's temperature are 220 DEG C, 8 area's temperature are 225 DEG C, 9 area's temperature are 230 DEG C, 10
Area's temperature is 230 DEG C.
(3) sheet material for squeezing out the second double screw extruder is by the sizing of three-roller calendaring system, most afterwards through cooling, Chu Bu,
Be prepared dynamic perduren waterproof roll finished product, the dynamic perduren waterproof roll of preparation with a thickness of 1mm, dynamic sulphur
Changing rubber water-proofing coiled width is 2000mm, and the length of dynamic perduren waterproof roll is 20m.
Comparative example 1
A kind of rubber water-proofing coiled preparation method, includes the following steps:
(1) it mediates: by 20 parts of ethylene propylene diene rubbers (EPDM), 20 parts of polyethylene (PE), 5 parts of maleic anhydride grafted polyethylenes
(MAH-g-PE), 10 parts of coumarone indene resins, 5 parts of naphthenic oils (KN-4010), 0.3 part of cumyl peroxide (DCP), 1 part 3 third
Alkenyl isocyanuric acid ester (TAIC), 0.5 part of nano zine oxide (ZnO), 1 part of stearic acid (SA), 8 parts of halogen-free flame retardants, 0.5 part
Co, 1 part of oxidized polyethylene wax (OPE wax), 1 part of silane coupling agent (KH-550), 1 part of antioxidant 1010,1 part of irgasfos 168,5
Part titanium dioxide is added in kneader or mediates in high-speed mixer, mixes, and kneading temperature control is at 85-90 DEG C, kneading time
For 5-6min, it is ensured that the above material dispersion is uniform；
(2) it is granulated: by the material after kneading by pelletizer mixing granulation, so that uniformly being divided between pellet and powder
It dissipates, double screw extruder extruder barrel temperature control is controlled when granulation at 150-180 DEG C, masterbatch is made；
(3) it extrusion calendaring: is squeezed out using double screw extruder plasticizing, then extruder barrel temperature control passes through at 150-180 DEG C
Tri-roll press machine calendering sizing, finally cool down, cutting and etc. be made polymer membranes.
Comparative example 2
A kind of preparation method of dynamic perduren waterproof roll, preparation process is substantially similar to embodiment 1, and difference exists
In the first double screw extruder extruder barrel temperature control of 1 first screw extruder of this comparative example is in 200-240 DEG C, net-changing device temperature
Degree control is controlled in 220 DEG C, metering pump temperature control in 220 DEG C, flange temperature 220 in 220 DEG C, the control of connection temperature
DEG C, mold temperature control at 225 DEG C, metering pump speed 7.0rad/min, screw speed 130-145r/min, the first twin-screw squeezes
Machine barrel temperature is segmented into that 1 area's temperature of barrel temperature is 200 DEG C, 2 area's temperature are 205 DEG C, 3 area's temperature are 210 DEG C, 4 area's temperature out
Degree is 210 DEG C, 5 area's temperature are 215 DEG C, 6 area's temperature are 220 DEG C, 7 area's temperature are 225 DEG C, 8 area's temperature are 230 DEG C, 9 area's temperature
For 235 DEG C, 10 area's temperature be 240 DEG C.
The dynamic perduren waterproof roll that 1,2,3 are prepared and the rubber that comparative example 1, comparative example 2 obtain will now be implemented
Glue waterproof roll carries out physical and chemical index test, and test result is shown in Table 1.
Table 1
From 1 data of table it is found that the waterproof that the preparation method of dynamic perduren waterproof roll provided by the invention is prepared
For coiled material compared with the common technique of the prior art, tensile strength, elongation at break and the tearing strength of product have obtained very great Cheng
The raising of degree, physicochemical property is more excellent, stable product quality, excellent fireproof performance；It is linked simultaneously with two double screw extruders,
Realize continuous production, product quality real time monitoring, and production technology production efficiency greatly improves, real-time online adjusts work
Skill, formula reduce rejection rate.From embodiment 1 and the comparison of comparative example 2 it is found that by strict control and adjusting double screw extruder
Each parameter, dynamic perduren waterproof roll comprehensive performance can be effectively ensured.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of preparation method of halogen-free flameproof dynamic perduren waterproof roll, which comprises the steps of:
(1) by rubber, thermoplastic resin, cosolvent, reinforcing agent, softening agent, the catalyst for accounting for catalyst total amount 10%-25%, help
Flow agent, the first double screw extruder is added in interface modifier, antioxidant, titanium dioxide, through plasticizing, shearing, be kneaded, be extruded into item and cut
Grain obtains being kneaded item, and at 170-210 DEG C, net-changing device temperature is controlled in 190-220 the first double screw extruder extruder barrel temperature control
DEG C, connection temperature control 190-220 DEG C, flange temperature control 190-220 DEG C, metering pump temperature control in 190-220
DEG C, mold temperature control in 190-220 DEG C, metering pump speed 5.0-12.0rad/min, screw speed 100-190 r/min；
(2) item will be kneaded to be added in the second double screw extruder, and is proportionally added into crosslinking agent, cross-linking aid, remaining catalysis
Agent, fire retardant complete dynamic vulcanization reaction by melting, mixing, exhaust, metering, and squeeze out semi-finished product sheet material, second pair of spiral shell
At 190-250 DEG C, the control of net-changing device temperature exists the control of bar extruder barrel temperature in 200-260 DEG C, connection temperature control
200-260 DEG C, flange temperature control 200-260 DEG C, metering pump temperature control 200-260 DEG C, mold temperature control exist
200-260 DEG C, metering pump speed 5.0-12.0 rad/min, screw speed 100-200r/min；
(3) it by the semi-finished product sheet material squeezed out through the second double screw extruder by calendering sizing, is most prepared into afterwards through cooling, deposit
To dynamic perduren waterproof roll finished product；
Wherein, each material is specific as follows: 20-30 parts of rubber；20-25 parts of thermoplastic resin；2-5 parts of cosolvent；Reinforcing agent
5-10 parts；5-10 parts of softening agent；5-10 parts of halogen-free flame retardants；0.3-1 parts of crosslinking agent；1-3 parts of cross-linking aid；Catalyst 2-
3.5 part；1-3 parts of glidant；1-3 parts of interface modifier；1-3 parts of antioxidant；5-10 parts of titanium dioxide.
2. preparation method according to claim 1, which is characterized in that the first double screw extruder barrel temperature segmentation
For 1 area's temperature of barrel temperature be 170-180 DEG C, 2 area's temperature are 175-185 DEG C, 3 area's temperature are 180-190 DEG C, 4 area's temperature are
180-195 DEG C, 5 area's temperature be 185-200 DEG C, 6 area's temperature are 190-195 DEG C, 7 area's temperature are 185-195 DEG C, 8 area's temperature are
190-200 DEG C, 9 area's temperature be 200-210 DEG C, 10 area's temperature are 210 DEG C.
3. preparation method according to claim 1, which is characterized in that the second double screw extruder barrel temperature segmentation
For 1 area's temperature of barrel temperature be 190-200 DEG C, 2 area's temperature are 195-205 DEG C, 3 area's temperature are 200-215 DEG C, 4 area's temperature are
205-220 DEG C, 5 area's temperature be 200-215 DEG C, 6 area's temperature are 195-215 DEG C, 7 area's temperature are 200-220 DEG C, 8 area's temperature are
200-225 DEG C, 9 area's temperature be 230-250 DEG C, 10 area's temperature are 230-250 DEG C.
4. preparation method according to claim 1, which is characterized in that the halogen-free flame retardants is phosphorus flame retardant and inorganic
The mixture of fire retardant.
5. the preparation method according to claim 4, which is characterized in that the halogen-free flame retardants be by surfactant at
The phosphorus flame retardant of reason and the mixture of inorganic fire retardants.
6. preparation method according to claim 1, which is characterized in that the rubber is ethylene propylene diene rubber and/or butyl
Rubber, wherein the ethylene contents of ethylene propylene diene rubber are 55%-75%.
7. preparation method according to claim 1, which is characterized in that the cosolvent is maleic anhydride, methacrylic acid
Ethylene oxidic ester, hydroxyethyl methacrylate grafted polyethylene, polypropylene or polyolefin elastomer.
8. preparation method according to claim 1, which is characterized in that the reinforcing agent be coumarone indene resin, Petropols,
One of phenolic resin, rosin resin are a variety of.
9. preparation method according to claim 1, which is characterized in that the softening agent is naphthenic oil and/or paraffin oil.
10. preparation method according to claim 1, which is characterized in that the crosslinking agent is cumyl peroxide, peroxide
Change one of two isobutylbenzenes, sulphur or a variety of.
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