CN102504394B - Production method of filled masterbatch formed through plasticization - Google Patents

Production method of filled masterbatch formed through plasticization Download PDF

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Publication number
CN102504394B
CN102504394B CN2011103624037A CN201110362403A CN102504394B CN 102504394 B CN102504394 B CN 102504394B CN 2011103624037 A CN2011103624037 A CN 2011103624037A CN 201110362403 A CN201110362403 A CN 201110362403A CN 102504394 B CN102504394 B CN 102504394B
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production method
added
plasticization
minutes
density polyethylene
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CN102504394A (en
Inventor
何和智
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And Chang (guangxi) Chemical Co Ltd
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And Chang (guangxi) Chemical Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/04Particle-shaped
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395Means 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
    • B29C48/40Means 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/92Measuring, controlling or regulating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92504Controlled parameter
    • B29C2948/92704Temperature
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92819Location or phase of control
    • B29C2948/92857Extrusion unit
    • B29C2948/92876Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895Barrel or housing

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

The invention relates to a production method of a filled masterbatch formed through plasticization. The filled masterbatch is composed of the following components in parts by weight: 5 to 16 parts of carrier resin, 3 to 8 parts of dispersant, 75 to 90 parts of inorganic filler, and 0.5 to 2 parts of surface-active agent. The production method comprises the following steps: stirring and mixing carrier resin and dispersants at a high speed, extruding and granulating the mixture of the carrier resin and dispersants by a co-rotating twin screw extrusion machine, and considering the mixture of the carrier resin and the dispersants as a standby material; stirring and mixing inorganic fillers, the surface-active agent and the standby material at a high speed, discharging and breaking the mixture of the inorganic fillers, the surface-active agent and the standby material, extruding and granulating the mixture of the inorganic fillers, the surface-active agent and the standby material by a co-rotating twin screw extrusion machine with the slenderness ratio: 32 to 48, cooling, and screening, finally obtaining the filled masterbatch. The packed masterbatch made through the production method is good in plasticization, the dispersion effect of the inorganic fillers is good, the whiteness is high, the requirement to the equipment is low, the energy consumption is low, and the yield is high.

Description

A kind of production method of filled masterbatch formed through plasticization
Technical field
The invention belongs to the master batch manufacturing technology field that inorganic powder combines with macromolecular material, be specifically related to a kind of production method of filled masterbatch formed through plasticization.
Background technology
The application of filling master batch in plastics can reduce the material cost of plastics, save synthetic resins, also have the characteristics such as the plastics of improvement physicals, raising working (machining) efficiency, formed in the whole nation and to have strengthened masterbatch with filling-modified, blend and take product as the leading factor, with the important emerging industry colony of the relevant combinations such as inorganic mineral filler, raw and auxiliary material, processing aid and special machinery manufacturing, it also is one of industry active, the most with fastest developing speed in the present Plastics Processing Industry.
Filler parent granule is a kind of more unmanageable material, and for reaching plasticizing fully, the mineral filler good dispersity is to the very high requirement of the mixing proposition of the plasticizing of molding device.At present, producing filler parent granule conventional process method is after first mineral filler being added the high mixer surface active, again with dispersion agent, processing aid and vector resin pre-mixing, at last by the dual-screw pelletizer extruding pelletization.For example, China Patent Publication No. is that CN101429686A discloses the good polymer master batch of a kind of dispersing property, and the concrete steps of its preparation are:
(1) the inorganic mineral powder finishing is processed: take by weighing inorganic mineral powder, place high-speed mixer, start and stir, rising temperature to 110 ℃ was kept 10 minutes, removed moisture; Then add coating materials, stirred 10 ~ 20 minutes; The test degree of activation reaches 100%, gets final product;
(2) the pre-dispersed processing of inorganic mineral powder: the inorganic mineral powder after step (1) finishing is placed kneader, add dispersion agent, be heated to 110 ~ 130 ℃, carry out pre-dispersed processing, 10 minutes time, rear cooling is pulverized;
(3) mixing, granulation: described pre-dispersed rear inorganic mineral powder is placed high-speed mixer, adds vector resin, start and stir, mixed 10 minutes, then, feed twin screw extruder, plastify, mixing, extrude, granulation; The processing condition of described twin screw extruder are: 160 ~ 196 ℃ of temperature, 200 ~ 500 rev/mins of screw speeds.
In this technique; the plasticizing of vector resin and the mixing effect of plasticizing that the coating of mineral filler is mainly relied on tablets press; tablets press is required height, usually all need the larger screw rod of length-to-diameter ratio and stronger screw combinations, just can produce and plastify filler parent granule complete, good dispersity.Therefore, this processing method is high to equipment requirements, energy consumption large, yield poorly, and the mixing effect of high-intensity plasticizing causes material degraded, variable color easily, affects the quality of filler parent granule.
Summary of the invention
The objective of the invention is the deficiency for the aforesaid method proposition, a kind of production method of filled masterbatch formed through plasticization is provided, the filler parent granule that this method makes plastifies, and the mineral filler dispersion effect is good, and whiteness is high, and low for equipment requirements, and energy consumption is little, and output is high.
The present invention is achieved by the following technical solutions:
A kind of production method of filled masterbatch formed through plasticization, its raw material consumption is counted by weight:
5 ~ 20 parts of vector resins
3 ~ 8 parts of dispersion agents
75 ~ 120 parts of mineral fillers
0.5 ~ 2 part of surfactant;
Comprise the steps:
(1) vector resin and dispersion agent are added in the high-speed mixer, stirred 2 minutes, in the compound adding parallel dual-screw extruding machine with gained, at 120 ~ 160 ℃ of lower extruding pelletizations, as standby material;
(2) mineral filler being added high-speed mixer stirs and is heated to 100 ~ 110 ℃, exhaust, again surfactant is added high-speed mixer, stirred 10 ~ 15 minutes, at last the prepared standby material of step (1) is added in the high-speed mixer and stirred 4 ~ 6 minutes, discharging, fragmentation namely obtains compound;
(3) step (2) gained compound being added length-to-diameter ratio is that at 140 ~ 180 ℃ of lower extruding pelletizations, cooling gets product after the screening in 32 ~ 48 the parallel dual-screw extruding machine.
The melting index of described vector resin is 2 ~ 7g/10min, and vector resin is one or more the combination in Low Density Polyethylene, linear low density polyethylene and the high density polyethylene(HDPE).
Described dispersion agent is one or more the combination in white oil, paraffin, polyethylene wax, oxidized polyethlene wax, stearic acid and stearic acid compound and the ethylene bis stearamide; Stearic acid compound
Described mineral filler is one or more compounds in calcium carbonate, talcum powder, barium sulfate and the Sodium sulfate anhydrous.min(99); The order number of mineral filler is 600 ~ 3000 orders.
Described surfactant is one or more combinations in stearic acid, silane coupling agent, titanate coupling agent, the aluminate coupling agent; Silane coupling agent is KH-550 or KH-570.
The invention has the beneficial effects as follows:
1, production method of the present invention can improve the plasticizing effect of filler parent granule, strengthens the dispersiveness of mineral filler.
2, existing method of producing master batch requires high to tablets press; usually all need the larger screw rod of length-to-diameter ratio and stronger screw combinations; just can produce and plastify filler parent granule complete, good dispersity; and the present invention is smaller to the wearing and tearing of production unit; can shorten the high-strength shear heat course in the material forming process; reduce the degraded of material, improve the quality of filler parent granule.
3, Raw of the present invention has passed through a pre-mixing through preplasticizing, thus when passing through tablets press again, low to the molding device requirement, do not need the very large screw rod of length-to-diameter ratio, reduce equipment loss, energy consumption is low, and output is high.
Specific embodiments
The present invention is described in further detail below in conjunction with embodiment, but embodiments of the present invention are not limited to the scope that embodiment represents.
Embodiment 1:
Feeding by weight: calcium carbonate 800 order 120kg, Low Density Polyethylene 8kg, linear low density polyethylene 4kg, paraffin 6kg, stearic acid 1kg.
Carry out as follows:
(1) with the 8kg Low Density Polyethylene, 4kg linear low density polyethylene, 6kg paraffin add in the high-speed mixer, start and stir, and stir 2 minutes, in the compound adding parallel dual-screw extruding machine with gained, at 140 ℃ of lower extruding pelletizations, as standby material;
(2) 120kg calcium carbonate is added high-speed mixer and stir and be heated to 110 ℃, exhaust adds high-speed mixer with the 1kg stearic acid again, stirred 15 minutes, and the prepared standby material of step (1) was added in the high-speed mixer stirred discharging 4 minutes at last, fragmentation namely obtains compound;
(3) step (2) gained compound being added length-to-diameter ratio is that at 160 ℃ of lower extruding pelletizations, cooling gets product after the screening in 36 the parallel dual-screw extruding machine.
In the granulation process, parallel dual-screw extruding machine forcing machine processing parameter:
Temperature Setting:
150℃、165℃、162℃、160℃、158℃、155℃、153℃、150℃、150℃
Screw speed: 320r/min.
Embodiment 2:
Feeding by weight: calcium carbonate 1250 order 120kg, Low Density Polyethylene 8kg, linear low density polyethylene 5kg, polyethylene wax 6kg, stearic acid 2kg, titanate coupling agent 1kg.
Carry out as follows:
(1). with the 8kg Low Density Polyethylene, 5kg linear low density polyethylene, 6kg polyethylene wax, the 2kg stearic acid adds in the high-speed mixer, starts and stirs, and stirs 2 minutes, the compound of gained is added in the parallel dual-screw extruding machine, at 120 ℃ of lower extruding pelletizations, as standby material;
(2). 120kg calcium carbonate is added the high-speed mixer stirring and is heated to 100 ℃, then exhaust is sprayed into the titanate coupling agent of 1kg while stirring, and high mixer continues to stir 10 minutes after the been sprayed, the material for making clothes that step (1) is prepared adds high mixer stirring 5 minutes, discharging again;
(3) step (2) gained compound being added length-to-diameter ratio is that at 180 ℃ of lower extruding pelletizations, cooling gets product after the screening in 36 the parallel dual-screw extruding machine.
In the granulation process, parallel dual-screw extruding machine forcing machine processing parameter:
Temperature Setting:
150℃、170℃、170℃、167℃、165℃、162℃、160℃、158℃、155℃
Screw speed: 250r/min
Embodiment 3:
By weight: barium sulfate 2500 order 120kg, Low Density Polyethylene 12kg, linear low density polyethylene 8kg, polyethylene wax 6kg, stearic acid 2kg, silane coupling agent 2kg.
Carry out as follows:
(1) with the 12kg Low Density Polyethylene, 8kg linear low density polyethylene, 6kg polyethylene wax, the 1kg stearic acid adds in the high-speed mixer, starts and stirs, and stirs 2 minutes, the compound of gained is added in the parallel dual-screw extruding machine, at 160 ℃ of lower extruding pelletizations, as standby material;
(2) 120kg barium sulfate being added high-speed mixer stirs and is heated to 100 ℃, exhaust, then be sprayed into while stirring the silane coupling agent of 1kg, high mixer continues to stir 12 minutes after the been sprayed, then adds the 1kg stearic acid, stirs 5 minutes, standby material with step (1) adds high-speed mixer stirring 6 minutes at last, discharging, fragmentation namely gets compound;
(3) the gained compound being added length-to-diameter ratio is 36 parallel dual-screw extruding machine extruding pelletizations, at 140 ℃ of lower extruding pelletizations, gets product behind the cooling, screening.
In the granulation process, parallel dual-screw extruding machine forcing machine processing parameter:
Temperature Setting:
150℃、165℃、170℃、170℃、168℃、168℃、165℃、162℃、160℃
Screw speed: 180r/min.
Embodiment 4:
Feeding by weight: Sodium sulfate anhydrous.min(99) 1250 order 120kg, Low Density Polyethylene 6kg, linear low density polyethylene 5kg, polyethylene wax 5kg, stearic acid 1.5kg, silane coupling agent 1kg.
Carry out as follows:
(1). with the 6kg Low Density Polyethylene, 5kg linear low density polyethylene, 5kg polyethylene wax, the 2kg stearic acid adds in the high-speed mixer, starts and stirs, and stirs 2 minutes, the compound of gained is added in the parallel dual-screw extruding machine, at 120 ℃ of lower extruding pelletizations, as standby material;
(2). the 120kg Sodium sulfate anhydrous.min(99) is added the high-speed mixer stirring and is heated to 100 ℃, then exhaust is sprayed into the silane coupling agent of 1kg while stirring, and high mixer continues to stir 10 minutes after the been sprayed, the material for making clothes that step (1) is prepared adds high mixer stirring 5 minutes, discharging again;
(3) step (2) gained compound being added length-to-diameter ratio is that at 180 ℃ of lower extruding pelletizations, cooling gets product after the screening in 36 the parallel dual-screw extruding machine.
In the granulation process, parallel dual-screw extruding machine forcing machine processing parameter:
Temperature Setting:
150℃、160℃、160℃、158℃、155℃、153℃、150℃、148℃、145℃
Screw speed: 300r/min.
Embodiment 5:
Feeding by weight: Sodium sulfate anhydrous.min(99) 1250 order 90kg, talcum powder 1250 order 30kg, Low Density Polyethylene 4kg, linear low density polyethylene 5kg, polyethylene wax 5kg, stearic acid 2kg, silane coupling agent 1kg.
Carry out as follows:
(1) with the 4kg Low Density Polyethylene, 5kg linear low density polyethylene, 5kg polyethylene wax, the 2kg stearic acid adds in the high-speed mixer, starts and stirs, and stirs 2 minutes, the compound of gained is added in the parallel dual-screw extruding machine, at 120 ℃ of lower extruding pelletizations, as standby material;
(2) talcum powder with 90kg Sodium sulfate anhydrous.min(99) and 30kg adds the high-speed mixer stirring and is heated to 100 ℃, exhaust, then be sprayed into while stirring the silane coupling agent of 1kg, high mixer continues to stir 10 minutes after the been sprayed, the material for making clothes that step (1) is prepared adds high mixer stirring 5 minutes, discharging again;
(3) step (2) gained compound being added length-to-diameter ratio is that at 180 ℃ of lower extruding pelletizations, cooling gets product after the screening in 36 the parallel dual-screw extruding machine.
In the granulation process, parallel dual-screw extruding machine forcing machine processing parameter:
Temperature Setting:
150℃、165℃、165℃、162℃、160℃、158℃、155℃、153℃、150℃
Screw speed: 240r/min.
Embodiment 6:
Feeding by weight: calcium carbonate 600 order 75kg, high density polyethylene(HDPE) 5kg, white oil 3kg, aluminate coupling agent 0.5kg.
Carry out as follows:
(1) with the 5kg high density polyethylene(HDPE), the 3kg white oil adds in the high-speed mixer, starts and stirs, and stirs 2 minutes, in the compound adding parallel dual-screw extruding machine with gained, at 150 ℃ of lower extruding pelletizations, as standby material;
(2) 75kg calcium carbonate being added high-speed mixer stirs and is heated to 105 ℃, exhaust, again the 0.5kg aluminate coupling agent is added high-speed mixer, stirred 13 minutes, at last the prepared standby material of step (1) is added in the high-speed mixer and stirred 5 minutes, discharging, fragmentation namely obtains compound;
(3) step (2) gained compound being added length-to-diameter ratio is that at 150 ℃ of lower extruding pelletizations, cooling gets product after the screening in 32 the parallel dual-screw extruding machine.
In the granulation process, parallel dual-screw extruding machine forcing machine processing parameter:
Temperature Setting:
150℃、165℃、162℃、160℃、158℃、155℃、153℃、150℃、150℃
Screw speed: 180r/min.
Embodiment 7:
Feeding by weight: Sodium sulfate anhydrous.min(99) 3000 order 80kg, talcum powder 3000 order 20kg, high density polyethylene(HDPE) 7kg, linear low density polyethylene 7kg, oxidized polyethlene wax 6kg, stearic acid 1.5kg, KH-550 1kg.
Carry out as follows:
(1) with the 7kg high density polyethylene(HDPE), 7kg linear low density polyethylene, 6kg oxidized polyethlene wax, 1.5kg stearic acid adds in the high-speed mixer, starts and stirs, and stirs 2 minutes, the compound of gained is added in the parallel dual-screw extruding machine, at 130 ℃ of lower extruding pelletizations, as standby material;
(2) 80kg Sodium sulfate anhydrous.min(99) and 20kg talcum powder are added the high-speed mixer stirring and be heated to 100 ℃, then exhaust is sprayed into the KH-550 of 1kg while stirring, and high mixer continues to stir 12 minutes after the been sprayed, the material for making clothes that step (1) is prepared adds high mixer stirring 5 minutes, discharging again;
(3) step (2) gained compound being added length-to-diameter ratio is that at 180 ℃ of lower extruding pelletizations, cooling gets product after the screening in 48 the parallel dual-screw extruding machine.
In the granulation process, parallel dual-screw extruding machine forcing machine processing parameter:
Temperature Setting:
150℃、160℃、160℃、158℃、155℃、153℃、150℃、148℃、145℃
Screw speed: 300r/min.

Claims (6)

1. the production method of a filled masterbatch formed through plasticization, it is characterized in that: its raw material consumption is counted by weight:
Figure FDA00003209529000011
Described vector resin is one or more the combination in Low Density Polyethylene, linear low density polyethylene and the high density polyethylene(HDPE);
Described dispersion agent is one or more the combination in white oil, paraffin, polyethylene wax, oxidized polyethlene wax, stearic acid and stearic acid compound and the ethylene bis stearamide;
Comprise the steps:
(1) vector resin and dispersion agent are added in the high-speed mixer, stirred 2 minutes, in the compound adding parallel dual-screw extruding machine with gained, at 120~160 ℃ of lower extruding pelletizations, as standby material;
(2) mineral filler being added high-speed mixer stirs and is heated to 100~110 ℃, exhaust, again surfactant is added high-speed mixer, stirred 10~15 minutes, at last the prepared standby material of step (1) is added in the high-speed mixer and stirred 4~6 minutes, discharging, fragmentation namely obtains compound;
(3) step (2) gained compound being added length-to-diameter ratio is that at 140~180 ℃ of lower extruding pelletizations, cooling gets product after the screening in 32~48 the parallel dual-screw extruding machine.
2. the production method of a kind of filled masterbatch formed through plasticization according to claim 1, it is characterized in that: the melting index of described vector resin is 2~7g/10min.
3. the production method of filled masterbatch formed through plasticization according to claim 1, it is characterized in that: described mineral filler is one or more compounds in calcium carbonate, talcum powder, barium sulfate and the Sodium sulfate anhydrous.min(99).
4. according to claim 1 or the production method of 3 described filled masterbatch formed through plasticizations, it is characterized in that: the order number of described mineral filler is 600~3000 orders.
5. the production method of filled masterbatch formed through plasticization according to claim 1, it is characterized in that: described surfactant is one or more combinations in stearic acid, silane coupling agent, titanate coupling agent, the aluminate coupling agent.
6. the production method of filled masterbatch formed through plasticization according to claim 5, it is characterized in that: described silane coupling agent is KH-550 or KH-570.
CN2011103624037A 2011-11-16 2011-11-16 Production method of filled masterbatch formed through plasticization Expired - Fee Related CN102504394B (en)

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CN101429686A (en) * 2008-12-11 2009-05-13 吴国铭 Polymer master batch with good dispersibility and its production method and application

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