CN102585319A - Vulcanizing system of brominated butyl rubber/ polypropylene thermoplastic elastomer sealing material and preparation method for sealing material - Google Patents
Vulcanizing system of brominated butyl rubber/ polypropylene thermoplastic elastomer sealing material and preparation method for sealing material Download PDFInfo
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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
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/58—Component parts, details or accessories; Auxiliary operations
- B29B7/72—Measuring, controlling or regulating
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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
- B29B7/00—Mixing; Kneading
- B29B7/80—Component parts, details or accessories; Auxiliary operations
- B29B7/88—Adding charges, i.e. additives
- B29B7/90—Fillers or reinforcements, e.g. fibres
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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
- B29B9/12—Making granules characterised by structure or composition
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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
- B29B9/12—Making granules characterised by structure or composition
- B29B9/14—Making granules characterised by structure or composition fibre-reinforced
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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
- B29C48/03—Extrusion 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
- B29C48/04—Particle-shaped
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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
- B29C48/36—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
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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
- B29B7/00—Mixing; Kneading
- B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
- B29B7/06—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices
- B29B7/10—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary
- B29B7/18—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with more than one shaft
- B29B7/183—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with more than one shaft having a casing closely surrounding the rotors, e.g. of Banbury type
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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
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
- B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
- B29B7/46—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft
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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
- B29B7/00—Mixing; Kneading
- B29B7/74—Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
- B29B7/7461—Combinations of dissimilar mixers
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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
- B29B9/04—Making granules by dividing preformed material in the form of plates or sheets
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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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Abstract
The invention provides a vulcanizing system of a brominated butyl rubber/ polypropylene thermoplastic elastomer sealing material and a preparation method for the sealing material. The vulcanizing system comprises a vulcanizing agent, a catalyst and an active agent. The vulcanizing agent is a sulfur-free vulcanizing system, is granular and dustless, and is easy to weigh, calculate and disperse and safe in operation. The preparation method is a dynamic vulcanizing blending method, and can comprise injection and extrusion molding; the cross-linked rubber phase is dispersed uniformly in a plastic phase; and the preparation method has the advantages of simple process, a small amount of waste, high production efficiency and the like. The performance of the prepared sealing material meets the requirement of national standard YBB00232004. The vulcanizing system can substitute brominated butyl vulcanized rubber and can be applied in various fields.
Description
Technical field
The present invention relates to thermoplastic elastomer, be specifically related to vulcanization system of a kind of brominated butyl rubber/polypropylene thermoplastic elastomer sealing material and preparation method thereof.
Background technology
Fast development along with pharmaceutical industries; Specification of quality to medicinal sealing material is also progressively improving; Medicinal sealing material by tree elastomer and butyl rubber preparation not only is easy to generate particle contamination, and has the problem of consistency with the encapsulation medicine, so day by day is eliminated.At present, the many medicine sealing materials of China manufacturing enterprise is being devoted to the research and development of brominated butyl rubber sealing material.Because brominated butyl rubber (IIR) is the elastomerics that butyl rubber makes through the bromination substitution reaction; Have saturated basically main chain; So have multifrequency nature; Except keeping characteristics such as the original low gas permeability of butyl rubber, high decay property, stability to aging, weather resisteant, ozone resistance and chemical proofing, also increased the not available following characteristic of conventional butyl rubbers: many, the good heat resistance of vulcanization.If adopt brominated butyl rubber to prepare medicinal sealing material, just can remedy the above-mentioned performance deficiency of tree elastomer and butyl rubber.One big characteristics of brominated butyl rubber can adopt multiple vulcanization system to vulcanize exactly, such as: sulfur vulcanization, amine sulfuration, peroxide vuleanization, morphine woods class (like DTDM) sulfuration, resin cure.When adopting resin cure, brominated butyl rubber uses low amounts of resin just just can vulcanize, and when requiring the sizing material of high stress at definite elongation, low compression set, its consumption can reach 7 parts, and general range of application is 1～7 part.
At present; The preparation technology of the medicinal sealing material of brominated butyl rubber is loaded down with trivial details; Need through operations such as mixing, the mold vulcanization of rubber and auxiliary agent and aftertreatments, and the double bond content of brominated butyl rubber main chain is very low, causes that its mold vulcanization speed is slow, production efficiency is low.Meanwhile, the scrap stock that produce in the production process are lost thermoplasticity because of vulcanization crosslinking, owing to not reusing the waste that causes material.
If can make full use of good processability, the advantages such as mechanical property is good, density is little, plasticity-of Vestolen PP 7052 (PP); Adopt IIR and Vestolen PP 7052 (PP) blend to prepare thermoplastic elastomer; Not only can be so that elastomerics have plasticity-, and can directly adopt injection molding technique to come preparing product.Therefore, complete processing is simple, and production efficiency is high, and prior thermoplastic elastic sealing material is to reuse, and saves material, has reduced the consumption of the energy widely.To the development of environmental protection and drug packages and sealing industry thereof be produced great pushing effect
Vestolen PP 7052 (PP) is a kind of crystalline polymer of compound with regular structure, is thermoplastic resin tasteless, nontoxic, light weight.It has following characteristics: 1. good processability, and good mechanical property, resistance toheat is good; 2. under no external force effect; 150 ℃ indeformable, and chemicalstability is good, acid-and base-resisting and organic solvent; Do not have an effect with most of pharmaceutical chemicalss (like nitrosonitric acid, chromic acid solution, halogen, benzene, tetracol phenixin, chloroform etc.), and suction hardly.3. have plasticity-, can process repeatedly.
Thermoplastic elastomer (TPE) is one type of novel high polymer material, and mechanical blending, dynamic part sulfuration and dynamic full vulcanization three phases have been experienced in the development of blending thermoplastic elastomer.So-called dynamic vulcanization is exactly to sneak into rubber in the thermoplastic resin matrix, in melting mixing, makes rubber highly cross-linked, makes crosslinked rubber become particulate (about 1 μ m) to be scattered in the resinous substrates and the method for system TPE.The gordian technique of preparation TPV is a dynamic vulcanization technology, and the thermoplastic elastomer that adopts dynamic vulcanization process to make is called TPV (TPV).TPV is a kind of specific type of thermoplastic elastomer (TPE), has than the better character of simple blend.This type of brominated butyl rubber/PP blending type thermoplastic elasticity is keeping many natural characteristicss of rubber phase; These characteristics comprise: green strength, vibration damping property, lower glass transition temperatures, and high-air-tightness, heat-resisting, anti-ozone, UV resistant irradiation and erosion resistance etc.
Therefore; Adopt a kind of feasible preparation method and suitable vulcanization system to improve the performance of butyl rubber/polypropylene thermoplastic elastomer, and realize that it is used as injection liquid and has certain practical value with otherwise purposes such as plug and sealing-ring, seal liners.
Summary of the invention
The technical problem that the present invention solves is vulcanization system that discloses a kind of brominated butyl rubber/polypropylene thermoplastic elastomer sealing material and preparation method thereof; Make and brominated butyl rubber/polypropylene thermoplastic elastomer process extruding-out process of preparation or the sealing material that injection molding process makes can be used for preparing goods such as drug packages, sealing-ring and sealing plug.This method at first open refine vulcanization system and brominated butyl rubber rubber unvulcanizate; On Banbury mixer, successively add Vestolen PP 7052, auxiliary agent, rubber unvulcanizate, vulcanization system then; Dynamic vulcanization makes brominated butyl rubber/polypropylene thermoplastic elastomer; Further sulfuration makes the TPV particle, through injection moulding or extruding-out process get final product brominated butyl rubber/polypropylene thermoplastic elastomer sealing material.
Brominated butyl rubber proposed by the invention/polypropylene thermoplastic elastomer sealing material is by the feedstock production that comprises following component and parts by weight: 100 parts of brominated butyl rubbers; 50～70 parts of Vestolen PP 7052; 50～100 parts of reinforcing fillers; 5～22 parts of vulcanization systems; 1～5 part of auxiliary agent; 1～1.5 part in oxidation inhibitor.
Described vulcanization system is no sulfur system, comprises 1～10 part of vulcanizing agent; 1～3 part of catalyzer; 3～9 parts in acvator.Wherein vulcanizing agent is the mixture of thermal-reactive alkyl phenolic resin/zinc oxide/IIR, and catalyzer is zinc chloride (ZnCl
2), acvator is zinc oxide (ZnO).
Described Vestolen PP 7052 is a COPP, and the consumption in sealing elastomer material is 50～70 weight parts; Described reinforcing filler is a calcinated argil, and the consumption in sealing elastomer material is 50～100 weight parts; Described auxiliary agent comprises tenderizer and lubricant, and wherein tenderizer is mainly whiteruss, and lubricant is mainly Triple Pressed Stearic Acid, polyethylene wax, and the consumption in sealing elastomer material is 1～5 weight part; Described oxidation inhibitor is Hinered phenols, is mainly four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010), and the consumption in sealing elastomer material is 1～1.5 weight part.
Vulcanization system of brominated butyl rubber of the present invention/polypropylene thermoplastic elastomer sealing material and preparation method thereof is specific as follows:
(1) accurate each proportioning component of weighing.
(2) begin to pratise down in the room temperature mill, add IIR, thermal-reactive alkyl phenolic resin, zinc oxide successively and make vulcanization system; In temperature is under 40～50 ℃, adds brominated butyl rubber, reinforcing filler, processing aid successively in two rollers are begun to pratise machine, and blend 10～12min obtains rubber unvulcanizate.
(3) be 60～90rpm at the closed-smelting machine rotor rotating speed, blending temperature is under 160～200 ℃ of conditions, adds Vestolen PP 7052 and auxiliary agent; Plasticizing 2～5min; Add the rubber unvulcanizate that step (2) makes then, blend 4～6min adds vulcanization system again; Dynamic vulcanization blend 4～8min makes brominated butyl rubber/polypropylene thermoplastic elastomer.Slice in mill is processed sheet material.Granulation is pulverized in the back, makes the TPV particle.
(4) adopt meshed double screw forcing machine in the same way, screw speed is 120～200r/min, and main rate of feeding is 30～50r/min; Head temperature is 170～200 ℃, and screw rod pan feeding section temperature is 120～170 ℃, and melting mixing section temperature is 180～230 ℃; Add the TPV particle that step (3) makes; Continue dynamic vulcanization and extrude, and granulation, make further sulfurized TPV particle.
(5) extrusion moulding and injection moulding, each section of forcing machine temperature is 140～200 ℃, and barrel zone temperature is 180～200 ℃ behind the injection moulding machine, and the front barrel temperature is 190～230 ℃, and injection pressure is 20～35MPa, and dwell pressure is 28～32MPa, and injection speed is 20～30cm
3Under/s the condition, add the TPV particle that step (4) makes, can make needed Industrial products respectively.
Prepared brominated butyl rubber/polypropylene thermoplastic elastomer the sealing material of the present invention has the following advantages:
Brominated butyl rubber of the present invention/polypropylene thermoplastic elastomer preparation technology compares with simple halogenated butyl rubber elastomer production technology; Adopted the complete processing of thermoplastics, it is simple to have a technological operation, and working condition is easy to control; Do not need molded vulcanization and aftertreatment; Scrap stock are few, save energy, productivity advantages of higher.The vulcanizing agent that the present invention uses is particulate state, and no dust is easy to weighing and calculating, is prone to disperse, and the no sulfur system of operational safety can well play sulfuration to brominated butyl rubber again simultaneously.Brominated butyl rubber/the polypropylene thermoplastic elastomer that makes has higher elongation at break; Excellent ageing-resistant, heat-resisting, low temperature resistant, chemicals-resistant, anti-ozone, water-fast and steam, oil resistant, fire-retardant and stronger performances such as rebound resilience; Meet in the present pharmaceutical industries the requirement of microbiotic Medical bottle stopper and other sealing materials thereof, can replace halogenated butyl rubber to be used as the application of aspects such as microbiotic Medical bottle stopper and medicinal sealing material.
The present invention adopts novel vulcanization system and novel dynamic vulcanization blending technology; And a kind of brominated butyl rubber/polypropylene thermoplastic elastomer sealing material that makes of working method of utilization thermoplastics; Compare with other halogenated butyl rubber/polypropylene thermoplastic elastomers and to have following advantage: tensile strength is big; Elongation at break is big, and compression set is little.Salient features is following:
Hardness (Shao Shi A): 40～85
100% tensile modulus: 2.0～9.0MPa
300% tensile modulus: 2.7～11.0MPa
Tensile strength: 4.5～11.5MPa
Elongation at break: 360～910%, reach as high as 910%
Tensile set: 10～80%
Embodiment
Combine specific embodiment that content of the present invention is carried out detailed explanation at present.
Embodiment 1
Material provided by the invention is formulated by weight proportion by following raw material:
Process by following process method:
(1) begins to pratise down in the room temperature mill, add IIR, thermal-reactive alkyl phenolic resin, zinc oxide successively and make vulcanization system; In temperature is under 40 ℃, adds brominated butyl rubber, calcinated argil successively, Yellow Protopet 2A, and processing aid, in two rollers were begun to pratise machine, blend 10min obtained rubber unvulcanizate.
(2) be 70rpm at the closed-smelting machine rotor rotating speed, blending temperature is under 180 ℃ of conditions, adds Vestolen PP 7052 and auxiliary agent; Plasticizing 2min adds the rubber unvulcanizate that makes, blend 4min then; Add vulcanization system again, dynamic vulcanization blend 6min makes brominated butyl rubber/polypropylene thermoplastic elastomer.Slice in mill is processed sheet material.
Brominated butyl rubber/polyacrylic the thermoplastic elastomer of above-mentioned process method preparation is pressed GB/T531-92, GB528-92 tested for hardness, tensile property, and test result is seen table 1:
The performance of table 1 brominated butyl rubber/polyacrylic thermoplastic elastomer sealing material
Embodiment 2
Material provided by the invention is formulated by weight proportion by following raw material:
More than each the prescription process by following process method:
(1) begins to pratise down in the room temperature mill, add IIR, thermal-reactive alkyl phenolic resin, zinc oxide successively and make vulcanization system; In temperature is under 40 ℃, adds brominated butyl rubber, reinforcing filler, processing aid successively in two rollers are begun to pratise machine, and blend 10min obtains rubber unvulcanizate.
(2) be 70rpm at the closed-smelting machine rotor rotating speed, blending temperature is under 180 ℃ of conditions, adds Vestolen PP 7052 and auxiliary agent; Plasticizing 2min adds the rubber unvulcanizate that makes, blend 4min then; Add vulcanization system again, dynamic vulcanization blend 6min makes brominated butyl rubber/polypropylene/olefin thermoplastic elastomer.Slice in mill is processed sheet material.
Brominated butyl rubber/polyacrylic the thermoplastic elastomer of above-mentioned process method preparation is pressed GB/T531-92, GB528-92 tested for hardness, tensile property, and test result is seen table 2:
Thermoplastic elastomer performance under the different sulphur-free vulcanization system of table 2 consumption
Embodiment 3
Material provided by the invention is formulated by weight proportion by following raw material:
Process by following process method:
(1) begins to pratise down in the room temperature mill, add IIR, thermal-reactive alkyl phenolic resin, zinc oxide successively and make vulcanization system; In temperature is under 40 ℃, adds brominated butyl rubber, reinforcing filler, processing aid successively in two rollers are begun to pratise machine, and blend 10min obtains rubber unvulcanizate.
(2) be 70rpm at the closed-smelting machine rotor rotating speed, blending temperature is under 180 ℃ of conditions, adds Vestolen PP 7052 and auxiliary agent; Plasticizing 2min adds the rubber unvulcanizate that makes, blend 4min then; Add vulcanization system again, dynamic vulcanization blend 6min makes brominated butyl rubber/polypropylene/olefin thermoplastic elastomer.Slice in mill is processed sheet material.
Brominated butyl rubber/polyacrylic the thermoplastic elastomer of above-mentioned process method preparation is pressed GB/T531-92, GB528-92 tested for hardness, tensile property, and test result is seen table 3:
The thermoplastic elastomer performance of table 3 different copolymer Vestolen PP 7052 preparation relatively
Embodiment 4
Material provided by the invention is formulated by weight proportion by following raw material:
At first, begin to pratise down, add IIR, thermal-reactive alkyl phenolic resin, zinc oxide successively, make the sulphur-free vulcanization system in the room temperature mill.
Secondly, in two roller mills in about 40 ℃ with brominated butyl rubber and calcinated argil, Yellow Protopet 2A, processing aid, MgO carries out mixing, obtains rubber unvulcanizate.
Take following three kinds of technological method for processing:
Technology one: in Banbury mixer, 180 ℃ of design temperatures are under the rotor speed 70rpm condition; Add COPP and antioxidant 1010, plasticizing 2min adds rubber unvulcanizate blend 4min; Add vulcanization system again, carry out dynamic vulcanization blend 6min, the blend that obtains is pressed into sheet; Granulation is pulverized in the back, makes the TPV particle.
Technology two: on Banbury mixer, connect the homophase twin screw extruder, setting homophase twin screw extruder screw speed is 160r/min, and main rate of feeding is 40r/min; Head temperature is 180 ℃, and screw rod pan feeding section temperature is 120 ℃, and melting mixing section temperature is 210 ℃; Add the TPV particle that technology one makes; Continue dynamic vulcanization and extrude,, obtain the TPV pellet again through the dicing machine pelletizing.
Technology three: in injection moulding machine, back barrel zone temperature is 180 ℃, and the front barrel temperature is 200 ℃, and injection pressure is 30MPa, and dwell pressure is 28MPa, and injection speed is 25cm
3Under the condition of/s, add the TPV pellet that technology two makes, injection molding.
The 3 groups of brominated butyl rubbers/polyacrylic thermoplastic elastomer of above-mentioned 3 kinds of complete processings preparation is pressed GB/T531-92, GB528-92 tested for hardness, tensile property, and test result is seen table 4:
Table 4 adopts the performance of different complete processing thermoplastic elastomers
Embodiment 5
Material provided by the invention is formulated by weight proportion by following raw material:
Process by following process method:
(1) begins to pratise down in the room temperature mill, add IIR, thermal-reactive alkyl phenolic resin, zinc oxide successively and make vulcanization system; In temperature is under 45 ℃, adds brominated butyl rubber, reinforcing filler, processing aid successively in two rollers are begun to pratise machine, and blend 12min obtains rubber unvulcanizate.
(2) be 70rpm at the closed-smelting machine rotor rotating speed, blending temperature is under 180 ℃ of conditions, adds Vestolen PP 7052 and auxiliary agent; Plasticizing 3min adds the rubber unvulcanizate that makes, blend 5min then; Add vulcanization system again, dynamic vulcanization blend 6min makes brominated butyl rubber/polypropylene/olefin thermoplastic elastomer.Slice in mill is processed sheet material.Granulation is pulverized in the back, makes the TPV particle.
(3) adopt meshed double screw forcing machine in the same way, screw speed is 160r/min, and main rate of feeding is 40r/min; Head temperature is 180 ℃, and screw rod pan feeding section temperature is 120 ℃, and melting mixing section temperature is 210 ℃; Add the TPV particle that step (2) makes; Continue dynamic vulcanization and extrude, and granulation, make further sulfurized TPV particle.
(4) injection moulding, barrel zone temperature is 180 ℃ behind the injection moulding machine, and the front barrel temperature is 200 ℃, and injection pressure is 30MPa, and dwell pressure is 28MPa, injection speed is 25cm
3Under/s the condition, add the TPV pellet that step (3) makes, make needed Industrial products.With reference to international standard YB00232004 the correlated performance of product is tested, test result is seen table 5.Scrap stock according to above-mentioned production technique produces carry out back mixing, and blend are pressed into sheet in about 150 ℃ in two roll rubber mixing mill, press GB/T531-92, GB528-92 tested for hardness, tensile property, and test result is seen table 6.
Table 5 brominated butyl rubber/polypropylene thermoplastic elastomer plug performance
The performance of table 6 back mixing glue
Can get, prepared brominated butyl rubber/polyacrylic thermoplastic elastomer has plasticity-, reprocesses little to its performance impact.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the present invention's design; Can also make some improvement and retouching, these improvement and retouching also should be regarded as in protection scope of the present invention.
Claims (8)
1. vulcanization system of brominated butyl rubber/polypropylene thermoplastic elastomer sealing material and preparation method thereof is characterized in that the preparation method of described brominated butyl rubber/polypropylene thermoplastic elastomer sealing material is following:
Batching: accurate each proportioning component of weighing.
Mixing: as under 40～50 ℃, brominated butyl rubber, reinforcing filler and auxiliary agent to be added in the blending equipment successively, behind blend 10～12min, make mixing materials.
Dynamic vulcanization: Vestolen PP 7052 and oxidation inhibitor are added in the blending equipment at 160～200 ℃; Fusion plastification; Add the blend of mixing materials high-temperature fusion behind 2～5min, add vulcanization system behind 4～6min, obtain brominated butyl rubber/polypropylene/olefin thermoplastic elastomer behind 4～8min.
Granulation: the brominated butyl rubber/polypropylene thermoplastic elastomer of gained in slice in mill, is processed sheet material.Granulation is pulverized in the back, makes the TPV particle.The TPV particle that makes is added further dynamic vulcanization of twin screw extruder and granulation.
Moulding: select extrusion moulding and injection molding according to product requirement.
Clean: to injection molding plug need under vacuum condition, clean, rinsing, drying, sterilization, oven dry, packaging final prod.
Do not need to clean for sealing-ring or sealed strip.
2. preparation method according to claim 1 and vulcanization system thereof is characterized in that the preparation feed composition of described brominated butyl rubber/polypropylene thermoplastic elastomer sealing material and parts by weight are: 100 parts of brominated butyl rubbers; 50～70 parts of Vestolen PP 7052; 50～100 parts of reinforcing fillers; 5～22 parts of vulcanization systems; 1～5 part of auxiliary agent; 1～1.5 part in oxidation inhibitor.
3. vulcanization system according to claim 1 is characterized in that vulcanization system is not have the stream vulcanization system, and vulcanizing agent is the mixture of thermal-reactive alkyl phenolic resin/zinc oxide/IIR, and its parts by weight are 1～10, and catalyzer is zinc chloride (ZnCl
2), its parts by weight are 1～3, and acvator is zinc oxide (ZnO), and its parts by weight are 3～9.
4. the preparation method of brominated butyl rubber according to claim 1/polypropylene thermoplastic elastomer sealing material; It is characterized in that selected Vestolen PP 7052 is a COPP; Reinforcing filler is a calcinated argil, and auxiliary agent comprises tenderizer and lubricant, and wherein tenderizer is mainly whiteruss; Lubricant is mainly Triple Pressed Stearic Acid, polyethylene wax, and the consumption in sealing elastomer material is 1～5 weight part; Oxidation inhibitor is Hinered phenols, is mainly four [β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010).
5. the preparation method of brominated butyl rubber according to claim 1/polypropylene thermoplastic elastomer sealing material is characterized in that selected blending equipment comprises mill, Banbury mixer, extruding granulator, extrusion shaping machine, injection moulding machine etc.
6. brominated butyl rubber according to claim 1/polypropylene thermoplastic elastomer preparation method, mixing used blending equipment is mill; The equipment of polyolefine and rubber master batch material melt blending is Banbury mixer, and processing condition are 60～90rpm for the closed-smelting machine rotor rotating speed, and blending temperature is 170～190 ℃.
7. the preparation method of brominated butyl rubber according to claim 1/polypropylene thermoplastic elastomer sealing material; It is characterized in that extruding and pelletizing process adopts meshed double screw forcing machine in the same way, its length-to-diameter ratio is 32～40, and processing condition are that screw speed is 120～200r/min; Main rate of feeding is 30～50r/min; Head temperature is 170～200 ℃, and screw rod pan feeding section temperature is 120～170 ℃, and melting mixing section temperature is 180～230 ℃.
8. the preparation method of brominated butyl rubber according to claim 1/polypropylene thermoplastic elastomer sealing material is characterized in that each section temperature is at 140～200 ℃ in the extrusion moulding; The Shooting Technique condition is 180～200 ℃ for the back barrel zone temperature, and the front barrel temperature is 190～230 ℃, and injection pressure is 20～35MPa, and dwell pressure is 28～32MPa, and injection speed is 20～30cm
3/ s.
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| CN104725732A (en) * | 2014-12-28 | 2015-06-24 | 山东道恩高分子材料股份有限公司 | Low-hardness medical thermoplastic brominated butyl rubber and preparation method thereof |
| CN105254936A (en) * | 2015-11-05 | 2016-01-20 | 徐州工业职业技术学院 | Rubber powder based material used for dynamically vulcanized thermoplastic elastomer (TPE) waterproof roll and preparation method thereof |
| CN106280500A (en) * | 2016-08-26 | 2017-01-04 | 广东省石油化工研究院 | A kind of thermoplastic dynamic vulcanized brombutyl/polypropene composition and preparation method thereof |
| CN107987407A (en) * | 2017-11-24 | 2018-05-04 | 广东省石油与精细化工研究院 | A kind of thermoplastic dynamic vulcanized BIIR/PP compositions and preparation method thereof |
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| CN103554577A (en) * | 2013-10-30 | 2014-02-05 | 无锡市威海达机械制造有限公司 | Ultrahigh-pressure sealing material |
| CN103554577B (en) * | 2013-10-30 | 2017-02-08 | 江苏贸隆机械制造有限公司 | Ultrahigh-pressure sealing material |
| CN104194172A (en) * | 2014-08-27 | 2014-12-10 | 安徽美祥实业有限公司 | Flame-retardant brominated butyl rubber material and preparation method thereof |
| CN104725732B (en) * | 2014-12-28 | 2017-05-24 | 山东道恩高分子材料股份有限公司 | Low-hardness medical thermoplastic brominated butyl rubber and preparation method thereof |
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| CN106280500A (en) * | 2016-08-26 | 2017-01-04 | 广东省石油化工研究院 | A kind of thermoplastic dynamic vulcanized brombutyl/polypropene composition and preparation method thereof |
| CN108864518A (en) * | 2017-05-16 | 2018-11-23 | 中国石油化工股份有限公司 | Antistatic brombutyl/polypropylene thermoplastic elastomer and combinations thereof and preparation method and application |
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| CN107987407B (en) * | 2017-11-24 | 2020-05-22 | 广东省石油与精细化工研究院 | Thermoplastic dynamic vulcanization BIIR/PP composition and preparation method thereof |
| CN109796689A (en) * | 2019-02-01 | 2019-05-24 | 青岛科技大学 | A kind of soft, can 3D printing brombutyl/polypropylene thermoplastic vulcanizate and its preparation method and application |
| CN110791031A (en) * | 2019-12-04 | 2020-02-14 | 北京橡胶工业研究设计院有限公司 | Low-hardness brominated butyl rubber polypropylene thermoplastic elastomer |
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| CN111040318B (en) * | 2019-12-31 | 2024-01-02 | 欧宝聚合物江苏有限公司 | Industrial production method of low-compression permanent deformation dynamic vulcanization TPV |
| CN111574779A (en) * | 2020-06-09 | 2020-08-25 | 山东京博中聚新材料有限公司 | Brominated butyl rubber/polypropylene thermoplastic elastomer composition containing attapulgite and preparation method thereof |
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