CN100404608C - Dynamic wholly vulcanized thermoplastic rubber one-step production process and apparatus - Google Patents

Dynamic wholly vulcanized thermoplastic rubber one-step production process and apparatus Download PDF

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CN100404608C
CN100404608C CNB2004100131023A CN200410013102A CN100404608C CN 100404608 C CN100404608 C CN 100404608C CN B2004100131023 A CNB2004100131023 A CN B2004100131023A CN 200410013102 A CN200410013102 A CN 200410013102A CN 100404608 C CN100404608 C CN 100404608C
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paraffin oil
vulcanization
dynamically
dcp
single stage
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CN1569947A (en
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施辉忠
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WUHAN GUDEWEI TECHNOLOGY DEVELOPMENT Co Ltd
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Abstract

The present invention relates to a process and an apparatus for producing fully-vulcanized thermoplastic rubber by one step, particularly to a thermoplastic elastomer material, which belongs to the field of macromolecular materials. The present invention has the technical scheme that the thermoplastic rubber comprises to 55% of EPDM, 15 to 60% of pp, 6 to 30% of paraffin oil and 3 to 15% of paraffin oil and DCP, wherein the main materials are stirred at high speed and are added in a melting mixing dynamic fully-vulcanized reaction machine according to proportion, large numbers of liquid vulcanized auxiliary agents are respectively and orderly filled in the dynamic melting mixing reaction machine via an auxiliary agent filling device according to proportion, the components are fully stirred, melted and mixed at the temperature of 160 DEG C to 180 DEG C to be dynamically and fully vulcanized, and uniformly dispersed to react to generate a thermoplastic rubber product, and the product is sent to a granulator to be prepared into a rubber product which is in the shape of granules. The apparatus used by the process has the advantages of simplicity, innovation and multiple functions, and prepares the product by one step. The process of the present invention has the advantages of energy saving, high product yield, high productive efficiency and stable quality.

Description

A kind of single stage method dynamic full-sulfuration thermoplastic rubber production technology and equipment
Technical field
The present invention's a kind of single stage method dynamic full-sulfuration thermoplastic rubber production technology and equipment belong to polymeric material field, particularly novel thermoplastic elastomer material.
Background technology
Rubber school class material is important macromolecular material, is widely used in national economy and each field of science and technology.Rubber need vulcanize processing and just have practicality, and traditional vulcanization of rubber processing belongs to thermosetting material processing, its complete processing complexity, the big and contaminate environment of labour intensity.Therefore, dynamic full-sulfuration thermoplastic rubber has caused people's very big interest, because this material had both had the elastic properties of rubber, has the easy machine-shaping characteristic of thermoplastic material again.
At present domestic have minority unit to relate to the dynamic full-sulfuration thermoplastic rubber production, but what adopt is multistep processes technology, generally is the molten amalgamation of rubber and plastic time, and a large amount liquid adjuvants need divide and add just dynamic vulcanizations for 2~3 times once.This multistep processes complex process, the energy consumption height, recovery rate is low, because of heating repeatedly, causes product performance fluctuation big (more than 15%), and per step is all lossy, so product yield is low.
External employing is on-line method at present, be actually the another kind of manifestation of multistep processes, promptly before the twin screw extruder of multistep processes, add and used a Banbury mixer, in Banbury mixer, finish the mixing of material, to join from the material that Banbury mixer comes out then and carry out vulcanization reaction the dual-screw-stem machine, and extruding pelletization, production is step.
Summary of the invention
In order to solve the problem that above-mentioned multistep processes and single stage method dynamic full-sulfuration thermoplastic rubber process and equipment exist, special one-step technology major ingredient of the present invention and vulcanization aid prescription and the processing condition of proposing, be particularly related to the composition and the ratio of a large amount liquid adjuvants, and according to arts demand based on twin screw extruder, dynamic full vulcanization reaction machine and corresponding adjuvants liquid and solid liquefaction injection device have been designed, to realize that the mixing major ingredient can be with in the disposable according to the order of sequence adding reaction of a large amount liquid adjuvants machine after adding the reaction machine, under the regulation processing condition, elastomeric material is evenly dispersed in the thermoplastics (PP) in dynamic down sulfuration and with molecule (less than 1um), and promptly single stage method is finished the production preparation of thermoplastic elastomer in this reaction machine.
Technical solution of the present invention is as follows:
1, a kind of single stage method dynamic full-sulfuration thermoplastic rubber production technology comprises composition of raw materials, and processing condition and the finished product are pressed following prescription:
Terpolymer EP rubber (EPDM) 30~55%
Polypropylene (PP) 15~60%
Paraffin oil 6~30%
Paraffin oil+dicumyl peroxide (DCP) 3~15%
Main raw material terpolymer EP rubber (EPDM) and polypropylene (PP) are pressed EPDM 30~55%; the ratio of PP15%~60%; mixed about 3~5 minutes through high-speed stirring; add in the dynamically molten vulcanization reaction machine that mixes up; again with the ratio of a large amount liquid curing auxiliary agent in paraffin oil 6~30% and paraffin oil+DCP 3~15%; mix through heating of vulcanization aid injection device and heat fused respectively; be injected into according to the order of sequence in the dynamically molten vulcanization reaction machine that mixes up; all component is in 160 °~180 ℃; through fully stirring molten mixing, dynamic full vulcanization and homodisperse reaction generate the thermoplastic elastomer product; again this product is delivered to tablets press, be prepared into particulate state thermoplastic elastomer product.
2, a kind of single stage method dynamic full-sulfuration thermoplastic of the present invention rubber production technology, said a large amount liquid curing auxiliary agent is pressed paraffin oil 6~30% and paraffin oil+DCP 3~5% jar heating in the heating of auxiliary agent injection device respectively, pass through valve, advance following jar of heating of heating, through microprocessor pump drive and coupler, keep 70 °~160 ℃ of liquid vulcanization aids, respectively through three inlets, add paraffin oil according to the order of sequence, paraffin oil and paraffin oil+DCP liquid mixture is to dynamically melting in the vulcanization reaction machine that mixes up.
3, a kind of single stage method dynamic full-sulfuration thermoplastic of the present invention rubber production technology, said vulcanization aid paraffin oil+DCP 3~15% mixtures, its two ratio DCP/ paraffin oil is 1/8-2.
4, a kind of single stage method dynamic full-sulfuration thermoplastic of the present invention rubber production technology, all batch ingredients is dynamically fully stirring in the molten vulcanization reaction machine that mixes up, and keeping reaction machine screw speed is 10~500 rev/mins.
5; single stage method dynamic full-sulfuration thermoplastic rubber production equipment of the present invention; comprise homogenizer (1); the dynamically molten vulcanization reaction machine (2) that mixes up; vulcanization aid injection device (3) and tablets press (4); said dynamically molten mix up vulcanization reaction machine (2) for fuselage long/directly (L/D) compare twin screw extruder greater than 52; be provided with major ingredient feeding cylinder (5); vulcanization aid inlet (6); its product exit end is communicated with tablets press (4); vulcanization aid injection device (3) is by agitator (9); in the heating jar (10), following jar (12) of valve (11) heating, microprocessor pump drive (13) and coupler (14) are formed.
6, single stage method dynamic full-sulfuration thermoplastic rubber production equipment of the present invention, the said dynamically major ingredient feeding cylinder (5) of the molten vulcanization reaction machine (2) that mixes up is arranged on fuselage one end, and at least three auxiliary agent sprues (6), (7), (8) are distributed in feeding cylinder (5) axis between fuselage 2/3 length.
7, a kind of single stage method dynamic full-sulfuration thermoplastic of the present invention rubber production equipment, the said dynamically molten vulcanization reaction machine (2) that mixes up has temperature-control device.
8, a kind of single stage method dynamic full-sulfuration thermoplastic of the present invention rubber production equipment is characterized in that jar (10) in the heating of said vulcanization aid injection device (3), heating following jar (12) and microprocessor pump drive all have temperature-control device.
9, a kind of single stage method dynamic full-sulfuration thermoplastic of the present invention rubber production equipment, the connection flexible pipe (15) by the band temperature-control device between the microprocessor pump drive (13) of said vulcanization aid injection device (3) and the coupler (14) connects.
Explained hereafter thermoplastic elastomer of the present invention adopts dynamically molten mix up vulcanization reaction machine and vulcanization aid injection device, equipment simply has innovation, integrate molten and mix, a large amount liquid adjuvants and add according to the order of sequence, that dynamic vulcanization disperses reaction etc. is multi-functional, realizes that single stage method finishes product preparation.This technology is saved the energy more than 50%, and the disposable adding technique of a large amount liquid adjuvants, realizes that disposable liquid addition reaches 50%.The product yield height, steady quality.And reduction labour intensity, improve work situation, help environment protection.
Description of drawings
The equipment synoptic diagram that Fig. 1, production technique of the present invention are used
Specific embodiments
Production technique of the present invention is finished full dynamic vulcanization and is made particle from being dosed into, and continuously carries out.The time length of material reaction process in present device and the size of output are mainly by feed intake quantity and adjust that screw speed realizes of control.
Existing bonding apparatus accompanying drawing illustrates the present invention:
Press major ingredient EPDM 43%, PP 18.5% gets material, stirred 3 minutes in homogenizer (1) high speed, through major ingredient feeding cylinder (5) it is added dynamically molten mixing in the vulcanization reaction machine, press paraffin oil 29.5% again, paraffin oil+DCP 9% ratio is got material, the agitator (9) that adds vulcanization aid injection device (3) respectively, jar (10) are heated to 100 ℃ through heating upward, by valve (11), enter heating following jar (12) and be heated to 100 ℃, make paraffin oil+DCP all melt-blended, through having temperature controlled microprocessor pump drive (13), pipe connecting (15) and coupler (14) inject reaction machine (2) according to the order of sequence with the liquid curing auxiliary agent.Witco 70 injects reaction machine (2) through vulcanization aid inlet (6), (7); paraffin oil+DCP liquid injects reaction machine (2) through vulcanization aid inlet (8); all the component material is in 170 °~180 ℃; reaction machine screw speed is 400 rev/mins; through fully stirring molten mixing, dynamic full vulcanization and homodisperse reaction; generate the thermoplastic elastomer product, again this product is delivered to tablets press (4) and be prepared into granular product.

Claims (9)

1. single stage method dynamic full-sulfuration thermoplastic rubber preparation method, its raw material is formed and proportioning is:
Terpolymer EP rubber (EPDM) 30~55%
Polypropylene (PP) 15~60%
Paraffin oil 6~30%
Paraffin oil+dicumyl peroxide (DCP) 3~15%
Main raw material terpolymer EP rubber (EPDM) and polypropylene (PP) are pressed EPDM 30~55%; the ratio of PP15%~60%; mixed 3~5 minutes through high-speed stirring; add in the dynamically molten vulcanization reaction machine that mixes up; again will be as the paraffin oil of liquid curing auxiliary agent and paraffin oil+DCP ratio in paraffin oil 6~30% and paraffin oil+DCP 3~15%; mix through heating of vulcanization aid injection device and heat fused respectively; be injected into according to the order of sequence in the dynamically molten vulcanization reaction machine that mixes up; all component is in 160 °~180 ℃; through fully stirring molten mixing; dynamic full vulcanization and homodisperse reaction; generate the thermoplastic elastomer product; again this product is delivered to tablets press, be prepared into particulate state thermoplastic elastomer product.
2. according to the said a kind of single stage method dynamic full-sulfuration thermoplastic rubber preparation method of claim 1, it is characterized in that the ratio in paraffin oil 6~30% and paraffin oil+DCP 3~15% as the paraffin oil of liquid curing auxiliary agent and paraffin oil+DCP, jar heating in the heating of auxiliary agent injection device respectively, pass through valve, advance following jar of heating of heating, through microprocessor pump drive and coupler, keep 70 ℃-160 ℃ of liquid vulcanization aids, respectively through three inlets, add paraffin oil according to the order of sequence, paraffin oil, and paraffin oil+DCP liquid mixture is to dynamically melting in the vulcanization reaction machine that mixes up.
3. according to claim 1 single stage method dynamic full-sulfuration thermoplastic rubber preparation method, in paraffin oil+dicumyl peroxide (DCP) 3~15% mixtures that it is characterized in that providing in raw material composition and proportioning, the DCP/ paraffin oil is 1/8-2.
4. according to the said a kind of single stage method dynamic full-sulfuration thermoplastic rubber preparation method of claim 1, it is characterized in that whole batch ingredients are dynamically fully stirring in the molten vulcanization reaction machine that mixes up, keeping reaction machine screw speed is 10~500 rev/mins.
5. single stage method dynamic full-sulfuration thermoplastic rubber production equipment of implementing the production method of claim 1; comprise homogenizer (1); the dynamically molten vulcanization reaction machine (2) that mixes up; vulcanization aid injection device (3) and tablets press (4); it is characterized in that dynamically molten mix up vulcanization reaction machine (2) for fuselage long/directly (L/D) compare twin screw extruder greater than 52; be provided with major ingredient feeding cylinder (5); vulcanization aid inlet (6); fully sulfurized thermoplastic rubber product exit end is communicated with tablets press (4); vulcanization aid injection device (3) is by agitator (9); in the heating jar (10); valve (11); heat following jar (12), microprocessor pump drive (13) and coupler (14) are formed.
6. according to the single stage method dynamic full-sulfuration thermoplastic rubber production equipment of claim 5, it is characterized in that the said dynamically major ingredient feeding cylinder (5) of the molten vulcanization reaction machine (2) that mixes up is arranged on fuselage one end, at least three auxiliary agent inlets (6), (7) and (8) are distributed in feeding cylinder (5) axis between fuselage 2/3 length.
7. according to the said single stage method dynamic full-sulfuration thermoplastic of claim 5 rubber production equipment, it is characterized in that the said dynamically molten vulcanization reaction machine (2) that mixes up has temperature-control device.
8. according to the said a kind of single stage method dynamic full-sulfuration thermoplastic rubber production equipment of claim 5, it is characterized in that jar (10) in the heating of said vulcanization aid injection device (3), heating following jar (12) and microprocessor pump drive all have temperature-control device.
9. according to the said single stage method dynamic full-sulfuration thermoplastic of claim 5 rubber production equipment, it is characterized in that the connection flexible pipe (15) by the band temperature-control device connects between the microprocessor pump drive (13) of said vulcanization aid injection device (3) and the coupler (14).
CNB2004100131023A 2004-04-29 2004-04-29 Dynamic wholly vulcanized thermoplastic rubber one-step production process and apparatus Expired - Fee Related CN100404608C (en)

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CN100400582C (en) * 2005-12-30 2008-07-09 四川省宜宾五粮液集团有限公司 Elastic cover material for container and production method thereof
DE102008040138A1 (en) * 2008-07-03 2010-01-07 Rhein Chemie Rheinau Gmbh Method and device for producing a crosslinkable rubber mixture
CN109627604A (en) * 2018-11-30 2019-04-16 河南大张过滤设备有限公司 A kind of diaphragm core material of corrosion-and high-temp-resistant
CN113248824B (en) * 2021-04-14 2022-09-20 山东道恩高分子材料股份有限公司 Preparation method of TPV (thermoplastic vulcanizate) tube material with high shear viscosity

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4130535A (en) * 1975-07-21 1978-12-19 Monsanto Company Thermoplastic vulcanizates of olefin rubber and polyolefin resin
WO2002018487A1 (en) * 2000-08-30 2002-03-07 Dsm N.V. Thermoplastic elastomer with improved low temperature properties

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4130535A (en) * 1975-07-21 1978-12-19 Monsanto Company Thermoplastic vulcanizates of olefin rubber and polyolefin resin
WO2002018487A1 (en) * 2000-08-30 2002-03-07 Dsm N.V. Thermoplastic elastomer with improved low temperature properties

Non-Patent Citations (2)

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Title
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动态硫化EPDM/PP共混型热塑性弹性体的研究. 郭红革等.橡胶工业,第45卷第4期. 1998 *

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