CN102443226B - Method for preparing halogen-free flame retardant PVC elastic material - Google Patents
Method for preparing halogen-free flame retardant PVC elastic material Download PDFInfo
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- CN102443226B CN102443226B CN2011102797626A CN201110279762A CN102443226B CN 102443226 B CN102443226 B CN 102443226B CN 2011102797626 A CN2011102797626 A CN 2011102797626A CN 201110279762 A CN201110279762 A CN 201110279762A CN 102443226 B CN102443226 B CN 102443226B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92904—Die; Nozzle zone
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- Mechanical Engineering (AREA)
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Abstract
The invention provides a halogen-free flame retardant PVC elastic material and a preparation method thereof, relating to a preparation method of a polymer composite material. The preparation method comprises the following steps of: mixing PVC resin in a kneader till the temperature is 70-80 DEG C; then adding a stabilizing agent, a plasticizer, a lubricant, pigments and a halogen-free flame retardant and continuing mixing till the temperature of the mixture is 85-95 DEG C and discharging the mixed material; cooling the mixed material in a cooling stirrer to 40-50 DEG C; and adding the cooled mixed material in a twin-screw extruder, and extruding strip-shaped halogen-free flame retardant PVC elastic material under the condition that the temperature of an extrusion die head is 130-150 DEG C. An elevator balance compensation chain sheath prepared from the special material provided by the invention has beautiful appearance, good toughness, good aging resistance, high thermal stability andgood fire retardant effect.
Description
Technical field
The present invention relates to a kind of technology of preparing of polymer composite, be specifically related to the preparation method that a kind of elevator balanced compensated chain sheath is used halogen-free flameproof PVC elastomerics PP Pipe Compound.
Background technology
Elevator balanced compensated chain is a kind of a kind of important safety parts that keep the smooth running of elevator lifting process.Elevator balanced compensated chain is by special-purpose welded chain cable and wrap up in matrix material outward and form, and for guarantee reduce friction noise, steadily of elevator balanced compensated chain in operational process, elevator balanced compensated chain must adopt have elastic polymer materials as the sheath of wrapping up in outward.Have elastic type of polymer a lot, comprise various thermoplastic elastomers and rubber.
Because PVC originates extensively, inexpensive, mechanical property is superior, and forming process is convenient, can make the PVC thermoplastic elastomer by modification.Due to the PVC thermoplastic elastomer poor fire of usually producing, easily produce toxic and harmful in combustion processes.
Summary of the invention
The object of the invention is to propose a kind of halogen-free flameproof PVC elastic material that can overcome the prior art present situation, have good environmental protection flame retardant.
The present invention is comprised of polyvinyl chloride resin, toughner, softening agent, stablizer, lubricant, halogen-free flame retardants and pigment; The weight ratio of described polyvinyl chloride resin, toughner, softening agent, stablizer, lubricant, halogen-free flame retardants and pigment is 100: 5～20: 40～80: 4～8: 1.5～3.5: 30～80: 0.3～1.0;
Wherein, described toughner is that chlorinity is 34～36% chlorinatedpolyethylene;
Described softening agent be by dioctyl phthalate (DOP) and diphenyl octyl phosphate with 4～10: 1 weight ratio is mixed the plastic binder that forms;
Described thermo-stabilizer is the non-toxic aq calcium zinc stabilizer;
Described lubricant is that stearic acid or molecular weight are 1000～5000 polyethylene wax;
Described halogen-free flame retardants is that median size is the modified aluminium hydroxide of 5～100 microns;
Described pigment is high-carbon black pigment.
The present invention has adopted two kinds of raw materials with environmental protection flame retardant function, and a kind of is the diphenyl octyl phosphate softening agent, and another kind is the micron order aluminium hydroxide fire retardant.Diphenyl octyl phosphate and micron order aluminium hydroxide have good fire-retardant synergy in the PVC elastomerics, can be reduced in simultaneously the generation of PVC elastomerics smoke density and obnoxious flavour in fire, elevator balanced compensated chain sheath by this pellet production has good environmental protection flame retardant, has also that Heat stability is good, cost are low, characteristics of easy extrusion moulding processing, good flame retardation effect.
Another purpose of the present invention is the production method that proposes halogen-free flameproof PVC elastic material.
Comprise the following steps:
1) polyvinyl chloride resin being placed in rotating speed is that the kneader of 800 rev/mins～1000 rev/mins is mixed to 70 ℃～80 ℃, add rear continuation to mix stablizer and softening agent again, then toughner, lubricant, pigment and halogen-free flame retardants are added and continue to mix, until the temperature of mixture reach 85 ℃～95 ℃ after discharging;
2) mixture is sent to is cooled to 40 ℃～50 ℃ in the cooling and stirring device;
3) cooled mixture being placed in twin screw extruder, is to extrude strip halogen-free flameproof PVC elastic material under the condition of 130 ℃～150 ℃ in the extrusion die temperature;
When feeding intake, the weight ratio of described polyvinyl chloride resin, toughner, softening agent, stablizer, lubricant, halogen-free flame retardants and pigment is 100: 5～20: 40～80: 4～8: 1.5～3.5: 30～80: 0.3～1.0;
Described toughner is that chlorinity is 34～36% chlorinatedpolyethylene;
Described softening agent be by dioctyl phthalate (DOP) and diphenyl octyl phosphate with 4～10: 1 weight ratio is mixed the plastic binder that forms;
Described thermo-stabilizer is the non-toxic aq calcium zinc stabilizer;
Described lubricant is that stearic acid or molecular weight are 1000～5000 polyethylene wax;
Described halogen-free flame retardants is that median size is the modified aluminium hydroxide of 5～100 microns;
Described pigment is high-carbon black pigment.
The present invention has positive effect: (1) the present invention adopts dioctyl phthalate (DOP) and diphenyl octyl phosphate to use in halogen-free flameproof PVC elastomerics PP Pipe Compound at the elevator balanced compensated chain sheath and forms compound Plasticising system, improve on the one hand the elastomeric lower temperature resistance of PVC, the more important thing is that diphenyl octyl phosphate also has the cooperative flame retardant effect, (2) in fire retardant of the present invention, the weight of coupling agent only accounts for 1%～3% of micron order aluminium hydroxide, reduced on the one hand production cost, the mobility that is conducive on the other hand the PVC melt is easy to extrusion moulding processing.(3) the present invention adopts aluminium hydroxide to make fire retardant, and the aluminium hydroxide thermolysis can produce water and aluminum oxide, plays smoke elimination, cooling, becomes the charcoal effect, is conducive to this PP Pipe Compound and has the environmental protection flame retardant effect.The elevator balanced compensated chain sheath outward appearance of (4) being produced by pellet of the present invention is good, good toughness, good (80 ℃ of heat-resistant aging, the tensile strength velocity of variation was less than 20% in 168 hours), thermally-stabilised height (200 ℃ of heat-stable times were greater than 60 minutes), good flame retardation effect (oxygen index is greater than 34).
Median size of the present invention is that the preparation method of the modified aluminium hydroxide of 5～100 microns is: to be the aluminium hydroxide of 5～100 microns and silane coupling agent be placed in rotating speed according to 100: 1～3 weight with median size is that the temperature that the mixing machine of 800 rev/mins～1000 rev/mins is mixed to mixture is 125 ℃～135 ℃, and then discharging is cooling gets final product;
The molecular structural formula of described silane coupling agent is Y-Si-(OR)
3, OR group wherein is alkoxyl group, and Y group is organo-functional group, and described organo-functional group is amino or methyl-prop acyloxy or vinyl.
In addition, twin screw extruder is divided into four heating zone and extrusion die according to the precedence of material process, and the Heating temperature of described four heating zone is followed successively by: T
1=90 ℃～110 ℃, T
2=110 ℃～120 ℃, T
3=120 ℃～130 ℃, T
4=130 ℃～150 ℃.
Embodiment
One, embodiment 1:
The elevator balanced compensated chain sheath of the present embodiment is with the halogen-free flameproof PVC elastomerics PP Pipe Compound co-mixing system that the additive in this polyvinyl chloride resin forms by polyvinyl chloride resin and blend.Additive comprises toughner, softening agent, stablizer, lubricant, fire retardant and pigment.Softening agent has two kinds, and the first is dioctyl phthalate (DOP), and the second is diphenyl octyl phosphate, and dioctyl phthalate (DOP) and diphenyl octyl phosphate are with 4～10: 1 weight ratio is mixed and is formed plastic binder.Use in halogen-free flameproof PVC elastomerics PP Pipe Compound at the elevator balanced compensated chain sheath of 232.8kg, each composition and content are as follows:
Polyvinyl chloride resin 100kg, toughner chlorinatedpolyethylene 12kg, thermo-stabilizer non-toxic aq calcium-zinc stabilizer 7kg, plasticizer phthalic acid dioctyl ester 50kg, the different monooctyl ester 10kg of phosphoric acid hexichol, lubricant stearic acid zinc 3.5kg, pigment carbon black 0.3kg, fire retardant Modified Micron level aluminium hydroxide 50kg.
Thermo-stabilizer derives from the non-toxic aq calcium-zinc stabilizer that the strong additives for plastics of Shanghai intelligence company limited produces.
The preparation method is:
1. prepare Modified Micron level aluminium hydroxide:
Take the silane coupling agent of the liquid state of the powdery micron order aluminium hydroxide of 100kg and 2.0kg, pouring micron order aluminium hydroxide and silane coupling agent into rotating speed is to mix in the high-speed mixer of 900 rev/mins, continue to stir 8min, the heat of friction that produces because of high-speed stirring makes temperature of charge be increased to 130 ℃, then discharging is cooling, namely obtain micron order aluminium hydroxide---the Modified Micron level aluminium hydroxide through the silane coupling agent processing as weighting agent, take 50kg from this Modified Micron level aluminium hydroxide, stand-by.
Above powdery micron order aluminium hydroxide refers to that median size is at the aluminium hydroxide of 5～100 microns.
Silane coupling agent is that the trade mark that Qufu morning twilight chemical industry company limited makes is the silane coupling agent of NQ-50.This silane coupling agent is to contain two kinds of different groups in a kind of molecule---the silica-based chemoattractant molecule of inorganic and organic reaction group.Its basic structure is Y-Si-(OR)
3, OR is the hydrolysable group alkoxyl group, as methoxyl group, oxyethyl group etc.Alkoxyl group can generate silanol with the reaction of moisture of calcium carbonate remained on surface, and the hydroxyl reaction of these silanols and surface of aluminum hydroxide generates alcoxyl structure and dehydration, forms firmly chemical bond.Y is organo-functional group, and as amino, methyl-prop acyloxy, vinyl etc., different organo-functional groups is applicable to different organic polymers, and it can or form physics winding, interpenetrating network system and form firmly chemical bond with polymer reaction.
Above-mentioned fire retardant can improve the consistency with the PVC matrix, and has suitably reduced production cost.The silane coupling agent macromolecular chain has good snappiness in addition, and co-mixing system is also had certain toughening effect.And if directly untreated micron order aluminium hydroxide is added in the PVC co-mixing system to the obvious mechanical strength that reduces this PP Pipe Compound of meeting.The micron order aluminium hydroxide of processing through silane coupling agent also has good processing fluidity.
2. take Modified Micron level aluminium hydroxide, the 3.5kg Zinic stearas of diphenyl octyl phosphate, the 50kg of dioctyl phthalate (DOP), the 10kg of liquid calcium-zinc stabilizer, the 50kg of toughner chlorinatedpolyethylene, the 7kg of S-1300 type polyvinyl chloride resin, the 12kg of 100kg, the carbon black of 0.3kg, stand-by.
3. first pouring the S-1300 type polyvinyl chloride resin that takes into rotating speed is to mix in 900 rev/mins of high-speed kneading machines, the heat of friction that produces because of high-speed stirring makes temperature of charge be increased to 75 ℃, again with the liquid calcium-zinc stabilizer, it is to continue in 900 rev/mins of high-speed mixers to mix that dioctyl phthalate (DOP) and diphenyl octyl phosphate are poured rotating speed into, then with the chlorinatedpolyethylene that takes, Zinic stearas, carbon black and Modified Micron level aluminium hydroxide pour into rotating speed be continue to mix in 900 rev/mins of high-speed mixers until the heat of friction that produces because of high-speed stirring make temperature of charge reach 90 ℃ after discharging, material is sent to is cooled to 40 ℃ in the cooling and stirring device.
4. material is sent into be heated to design temperature in twin screw extruder, mixture is in the process process of twin screw extruder, be heated on the one hand and softening and become molten state gradually, various compositions further evenly mix at the volley on the other hand, extruded into strips by die head at last, (particle diameter is about 2mm～3mm) and namely obtains the elevator balanced compensated chain sheath with halogen-free flameproof PVC elastomerics PP Pipe Compound to adopt fervent mode granulation when extruding; The extrusion die temperature T that sets
Mould=140 ℃.Twin screw extruder is divided into 4 heating zone and extrusion die according to the precedence of material process, and the Heating temperature of each heating zone that sets is followed successively by: T
1=90 ℃～110 ℃, T
2=110 ℃～120 ℃, T
3=120 ℃～130 ℃, T
4=130 ℃～150 ℃, the temperature of extrusion die is T=130 ℃～150 ℃.
The PP Pipe Compound that the present invention forms is made the elevator balanced compensated chain sheath, and its performance test sees Table 1.
Two, embodiment 2:
The rest part of the present embodiment is identical with embodiment 1, and difference is: use in halogen-free flameproof PVC elastomerics PP Pipe Compound at the elevator balanced compensated chain sheath of 232.8kg, each composition and corresponding content are as follows:
Polyvinyl chloride resin 100kg, toughner chlorinatedpolyethylene 17kg, thermo-stabilizer non-toxic aq calcium-zinc stabilizer 7kg, plasticizer phthalic acid dioctyl ester 45kg, the different monooctyl ester 10kg of phosphoric acid hexichol, lubricant stearic acid zinc 3.5kg, pigment carbon black 0.3kg, fire retardant Modified Micron level aluminium hydroxide 50kg.
Step 2. in, the weight of the various raw materials that take is corresponding with the content of above-mentioned each composition, also namely take Modified Micron level aluminium hydroxide, the 3.5kg Zinic stearas of diphenyl octyl phosphate, the 50kg of dioctyl phthalate (DOP), the 10kg of liquid calcium-zinc stabilizer, the 45kg of toughner chlorinatedpolyethylene, the 7kg of S-1300 type polyvinyl chloride resin, the 17kg of 100kg, the carbon black of 0.3kg, stand-by.
The PP Pipe Compound that the present invention forms is made the elevator balanced compensated chain sheath, and its performance test sees Table 1.
Three, embodiment 3:
The rest part of the present embodiment is identical with embodiment 1, and difference is: use in halogen-free flameproof PVC elastomerics PP Pipe Compound at the elevator balanced compensated chain sheath of 246.3kg, each composition and corresponding content are as follows:
Polyvinyl chloride resin 100kg, toughner chlorinatedpolyethylene 15kg, thermo-stabilizer non-toxic aq calcium-zinc stabilizer 7kg, plasticizer phthalic acid dioctyl ester 50kg, the different monooctyl ester 10kg of phosphoric acid hexichol, lubricant stearic acid zinc 4kg, pigment carbon black 0.3kg, fire retardant Modified Micron level aluminium hydroxide 60kg.
Corresponding, when the above-mentioned elevator balanced compensated chain sheath of preparation is used halogen-free flameproof PVC elastomerics PP Pipe Compound, step 2. in, the weight of the various raw materials that take is corresponding with the content of above-mentioned each composition, also namely take Modified Micron level aluminium hydroxide, the 4kg Zinic stearas of diphenyl octyl phosphate, the 60kg of dioctyl phthalate (DOP), the 10kg of liquid calcium-zinc stabilizer, the 50kg of toughner chlorinatedpolyethylene, the 7kg of S-1300 type polyvinyl chloride resin, the 15kg of 100kg, the carbon black of 0.3kg, stand-by.
The PP Pipe Compound that the present invention forms is made the elevator balanced compensated chain sheath, its performance test table 1.
Four, embodiment 4:
The rest part of the present embodiment is identical with embodiment 1, and difference is: use in halogen-free flameproof PVC elastomerics PP Pipe Compound at the elevator balanced compensated chain sheath of 252.3kg, each composition and corresponding content are as follows:
Polyvinyl chloride resin 100kg, toughner chlorinatedpolyethylene 12kg, thermo-stabilizer non-toxic aq calcium-zinc stabilizer 7kg, plasticizer phthalic acid dioctyl ester 60kg, the different monooctyl ester 10kg of phosphoric acid hexichol, lubricant stearic acid zinc 3kg, pigment carbon black 0.3kg, fire retardant Modified Micron level aluminium hydroxide 60kg.
Corresponding, when the above-mentioned high-impact pipe member pellet of preparation, step 2. in, the weight of the various raw materials that take is corresponding with the content of above-mentioned each composition, also namely take Modified Micron level aluminium hydroxide, the 3kg Zinic stearas of diphenyl octyl phosphate, the 60kg of dioctyl phthalate (DOP), the 10kg of liquid calcium-zinc stabilizer, the 60kg of toughner chlorinatedpolyethylene, the 7kg of S-1300 type polyvinyl chloride resin, the 12kg of 100kg, the carbon black of 0.3kg, stand-by.
The PP Pipe Compound that the present invention forms is made the elevator balanced compensated chain sheath, its performance test table 1.
Table 1
| Test performance | Performance index | Testing standard | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Tensile strength/MPa | ﹥9.5 | GB/T1043-2006 | 10.6 | 11.0 | 10.2 | 9.9 |
| Elongation at break/% | ﹥300 | GB/T1043-2006 | 400 | 350 | 420 | 450 |
| Thermal ageing (80 ℃, 168 hours) tensile strength velocity of variation/% | ≤20 | ? | 15.2 | 17.3 | 16.4 | 16.1 |
| 200 ℃ of heat-stable time/h | ≥60 | GB 2917-82 | 71.6 | 72.1 | 72.5 | 72.2 |
| The ballistic method embrittlement temperature/℃ | ≤-35 | GB/T5470-2008 | 40 | 41 | 42 | 45 |
| Oxygen index/% | ﹥34 | GB/T2406.2-2009 | 37 | 37 | 38 | 38 |
| Shore hardness | 60±5 | GB2411-2008 | 62 | 62 | 64 | 63 |
By as seen from Table 1, the PP Pipe Compound that adopts the present invention to make is made the elevator balanced compensated chain sheath, the requirement that all conforms to current standards of its indices, outward appearance is good, good toughness, good (80 ℃ of heat-resistant aging, the tensile strength velocity of variation was less than 20% in 168 hours), thermally-stabilised height (200 ℃ of heat-stable times were greater than 60 minutes), good flame retardation effect (oxygen index is greater than 34).
Claims (3)
1. the production method of a halogen-free flameproof PVC elastic material is characterized in that comprising the following steps:
1) polyvinyl chloride resin being placed in rotating speed is that the kneader of 800 rev/mins～1000 rev/mins is mixed to 70 ℃～80 ℃, add rear continuation to mix stablizer and softening agent again, then toughner, lubricant, pigment and halogen-free flame retardants are added and continue to mix, until the temperature of mixture reach 85 ℃～95 ℃ after discharging;
2) mixture is sent to is cooled to 40 ℃～50 ℃ in the cooling and stirring device;
3) cooled mixture being placed in twin screw extruder, is to extrude strip halogen-free flameproof PVC elastic material under the condition of 130 ℃～150 ℃ in the extrusion die temperature;
When feeding intake, the weight ratio of described polyvinyl chloride resin, toughner, softening agent, stablizer, lubricant, halogen-free flame retardants and pigment is 100: 5～20: 40～80: 4～8: 1.5～3.5: 30～80: 0.3～1.0;
Described toughner is that chlorinity is 34～36% chlorinatedpolyethylene;
Described softening agent be by dioctyl phthalate (DOP) and diphenyl octyl phosphate with 4～10: 1 weight ratio is mixed the plastic binder that forms;
Described stablizer is the non-toxic aq calcium zinc stabilizer;
Described lubricant is that stearic acid or molecular weight are 1000～5000 polyethylene wax;
Described halogen-free flame retardants is that median size is the modified aluminium hydroxide of 5～100 microns;
Described pigment is high-carbon black pigment.
2. the production method of halogen-free flameproof PVC elastic material according to claim 1, it is characterized in that described median size is that the preparation method of the modified aluminium hydroxide of 5～100 microns is: to be the aluminium hydroxide of 5～100 microns and silane coupling agent be placed in rotating speed according to 100: 1～3 weight with median size is that the temperature that the mixing machine of 800 rev/mins～1000 rev/mins is mixed to mixture is 125 ℃～135 ℃, and then discharging is cooling gets final product;
The molecular structural formula of described silane coupling agent is Y-Si-(OR)
3, OR group wherein is alkoxyl group, and Y group is organo-functional group, and described organo-functional group is amino or methyl-prop acyloxy or vinyl.
3. the production method of described halogen-free flameproof PVC elastic material according to claim 1 and 2, is characterized in that twin screw extruder is divided into four heating zone and extrusion die according to the precedence of material process, and the Heating temperature of described four heating zone is followed successively by: T
1=90 ℃～110 ℃, T
2=110 ℃～120 ℃, T
3=120 ℃～130 ℃, T
4=130 ℃～150 ℃.
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