CN105885258A - Low-pressure deformation chlorosulfonated rubber composite material and preparation method thereof - Google Patents
Low-pressure deformation chlorosulfonated rubber composite material and preparation method thereof Download PDFInfo
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- CN105885258A CN105885258A CN201410491276.4A CN201410491276A CN105885258A CN 105885258 A CN105885258 A CN 105885258A CN 201410491276 A CN201410491276 A CN 201410491276A CN 105885258 A CN105885258 A CN 105885258A
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Abstract
The invention discloses a low-pressure deformation chlorosulfonated rubber composite material. The rubber composite material comprises, by mass, 70-90 parts of chlorosulfonated polyethylene rubber, 10-30 parts of an ethylene propylene diene monomer, 3-6 parts of a homogeneous agent, 10-20 parts of an active agent, 2-5 parts of a processing assistant, 40-60 parts of a reinforcing agent, 10-20 parts of a plasticizer and 6-10 parts of a vulcanizing agent. The low-pressure deformation chlorosulfonated rubber composite material solves the technical problem of large high temperature compression permanent deformation of chlorosulfonated rubber. The preparation method is convenient for processing. The composite material has a low price and considerable economic benefits.
Description
Technical field
The present invention relates to rubber composite preparation field, more specifically, be a kind of low buckling chlorosulfonation
Rubber composite and preparation method thereof.
Background technology
Rubber seal products is the staple product that a class relates to China's national defense construction and economic construction,
Space flight, aviation, boats and ships, machinery, automobile and transportation, petrochemical industry, medicine, food and domestic
The range of application of the industries such as electrical equipment is more and more extensive, and rubber seal products has become the basic courses department of all trades and professions
Part or important accessory.Along with economic develops rapidly, scarcity of resources and the enhancing of environmental consciousness, to rubber
The serviceability of sealing article, reliability and life-span have higher requirement, and especially auto industry is sent out
Generated is mainstay of the national economy industry, and great impetus is played in the development to rubber seal products.
Hyundai Motor pursues high speed and comfortableness, to rubber seal products such as oil sealing, rubber o-ring, abnormal shape
The sealing property of sealing member etc. proposes tightened up requirement.
The compression set of rubber packing material is the lowest, and the sealing property of goods is the best.Compression is permanent to be become
Shape value characterizes elastomeric material expendable deformation quantity under load, is that quantitative description is elastic
The body retention time under long-term load, is the very important sign of material seal.Vulcanite passes through
The effect of compression stress, when, after stress relieving, some deformation of vulcanite cannot recover, claims
For permanent deformation.When compression set increases to certain value, rubber seal can occur lubricating oil to let out
The phenomenons such as leakage, and then cause the decline of sealing property, make goods lose use value.Thus compression is permanent
The size of deformation is one of important indicator weighing rubber sealing property quality and length in service life.
Therefore, how research improves the sealing property of rubber seal products or affects vulcanite compression set
Various factors become an important topic of rubber manufacturing enterprise and research department, have important
Practical value and economic worth.Such as patent CN 101831270.A has invented one and has had low compression set
The polysulfide caulking gum of deformation, compared with before modified, its mechanical property is held essentially constant, but compression is forever
Deformation for a long time significantly reduces.This patent is mainly by introducing a small amount of benzene ring structure in polysulfide strand, has
Effect prevents polysulfide strand from breakking away, and improves caulking gum anti-compression properties and reduces Compression Set.
Patent CN101338047A has invented the cold tolerant butadiene nitrile rubber combination of a kind of low rigidity, low contracting permanent deformation
Thing.Balance the tolerance to cold of rubber seal product, oil resistivity and low compression set performance well.
Patent CN 101875750A discloses a kind of low compression set fluororubber compounded rubber and preparation method thereof.
Improve the sealing property of non-perfluorinated rubber, i.e. reduce the compression set performance of fluorubber so that it is be full
Foot seals the requirement of industry goods.Patent CN 102731862A discloses one and has low compression set change
The rubber composition of shape characteristic, it is by nitrile rubber 3345, neoprene, anti-aging agent RD, prevents old
Agent MB, the raw material such as stearic acid is made.And about the patent of chlorosulfonation rubber low compression set and document
Report is few.
More come to meet in plant equipment production process the permanent set at high temperature to rubber seal product
The highest requirement, solves in production application because rubber seal compression set is big thus causes sealing
The problems such as effect is undesirable and service life is short, a kind of low buckling chlorosulfonation rubber of invention is multiple
Condensation material and preparation method thereof.
Summary of the invention
Owing to prior art also exists the problems referred to above, it is rubber combined that the present invention proposes a kind of low buckling chlorosulfonation
Material and preparation method thereof, in order to meet in plant equipment production process the high-temperature high-pressure to rubber seal product
The requirement that compression permanent deformation is the highest, solves in production application because of rubber seal Compression Set
Big thus cause sealing effectiveness undesirable and the problem such as service life is short.
The present invention solves the problems referred to above by the following technical programs:
A kind of low buckling chlorosulfonation rubber composite, each component under including mass fraction being: chlorosulfonation
Polyethylene rubber 70-90 part, ethylene propylene diene rubber 10-30 part, homogeneous agent 3-6 part, activating agent 10-20
Part, processing aid 2-5 part, reinforcing agent 40-60 part, plasticizer 10-20 part, vulcanizing agent 6-10 part.
The Mooney viscosity ML of described CSM1+4Control at 50-60 under 100 DEG C of test conditions
Between, its chlorine mass content is 35%;And the mass content of described ethylene propylene diene rubber is 7-8%.
Described homogeneous agent is anime mixture.
Described activating agent is extra light calcined magnesia, and its iodine number is more than 150.
Described processing aid is halogen-absorber and fatty acid and the mixture of derivant thereof, and described
The ratio of halogen-absorber and fatty acid and derivant thereof is 0: 1-1: 0.
Described halogen-absorber is one of zinc stearate, magnesium stearate, calcium stearate, synthetic hydrotalcite.
Described fatty acid and derivant thereof are stearic acid, stearic amide, N, the double hard amide of N '-ethylene
One of.
Described reinforcing agent is the mixing of any one or both in middle particle ardent method white carbon black or modified barium sulphate
Thing, and the mesh number of described modified barium sulphate is more than 4000 mesh.
Described plasticizer is polyesters plasticizer, and described plasticizer is polyadipate fourth diester, gathers pungent two
One of dibutyl phthalate or its complex.
Described vulcanizing agent is peroxide initiator and maleimide paralled system, and wherein said Malaysia
Imido mass fraction is no less than 1.5 parts.
Described peroxide initiator is peroxide diisopropylbenzene (DIPB).
Present invention also offers the preparation method of a kind of buckling chlorosulfonation rubber composite, including walking as follows
Rapid:
1. banbury processing is used, first by CSM, ethylene propylene diene rubber and homogeneous
Refining 8-10 minute is closed in agent under the conditions of 120-130 DEG C, parks 72 hours after discharge under room temperature;
2. premixing glue is put into again banbury pressing 2 minutes, adds activating agent, processing aid, reinforcement
Agent and mixing 6-8 minute of plasticizer, dump temperature controls between 110-120 DEG C, parks 24 hours
Above;
Add vulcanizing agent the most on a mill until mixing uniformly, thin logical 3 times of 0.5mm roll spacing, 4mm roll spacing bottom sheet
Cooling;
4. vulcanizing, its vulcanization parameters is first cure temperature 170 DEG C, and cure time is 15 minutes;
Second segment curing temperature is 150 DEG C, and cure time is 2 hours.
Low buckling chlorosulfonation rubber composite of the present invention and preparation method thereof has the advantage that
First, this rubber composite solves the technology that the high temperature compressed permanent deformation of chlorosulfonation rubber is big
A difficult problem;
Second, the preparation technology of the present invention and process very convenient;
3rd, the composite that the present invention obtains is cheap, economic benefits.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further elaborated.
Comparative example 1:
In banbury, 1000g ethylene propylene diene rubber is closed under the conditions of 125 DEG C refining 10 minutes, discharge
72 hours are parked under rear room temperature;Premixing glue is put into again banbury pressing 2 minutes, adds 150g oxygen
Change magnesium, 30g stearic acid, 500g white carbon black and 150g poly-suberic acid dibutyl ester, mixing 8 minutes, discharge
Temperature controls between 110-120 DEG C, parks more than 24 hours, adds 80g vulcanizing agent on a mill until
Mixing uniformly, thin logical 3 times of 0.5mm roll spacing, 4mm roll spacing bottom sheet cools down.Its vulcanization parameters is first
Section curing temperature 170 DEG C, cure time is 15 minutes;Second segment curing temperature is 150 DEG C, cure time
It it is 2 hours.
Comparative example 2:
In banbury, 1000g CSM is closed under the conditions of 125 DEG C refining 10 minutes,
Park under room temperature 72 hours after discharge;Premixing glue is put into again banbury pressing 2 minutes, adds
150g magnesium oxide, 30g stearic acid, 500g white carbon black and mixing 8 minutes of 150g poly-suberic acid dibutyl ester,
Dump temperature controls between 110-120 DEG C, parks more than 24 hours, adds 80g sulfur on a mill until
Agent is mixing uniformly, and thin logical 3 times of 0.5mm roll spacing, 4mm roll spacing bottom sheet cools down.Its vulcanization parameters is
First cure temperature 170 DEG C, cure time is 15 minutes;Second segment curing temperature is 150 DEG C, sulfuration
Time is 2 hours.
Comparative example 3:
In banbury, by 800g CSM, ethylene propylene diene rubber 200g is at 125 DEG C
Under the conditions of close refining 10 minutes, park under room temperature 72 hours after discharge;Premixing glue is put into again banbury
Pressing 2 minutes, adds 150g magnesium oxide, 30g stearic acid, 500g white carbon black and the poly-suberic acid of 150g
Mixing 8 minutes of dibutyl ester, dump temperature controls between 110-120 DEG C, parks more than 24 hours,
Adding 80g vulcanizing agent in mill mixing uniformly, thin logical 3 times of 0.5mm roll spacing, 4mm roll spacing bottom sheet is cold
But.Its vulcanization parameters is first cure temperature 170 DEG C, and cure time is 15 minutes;Second segment
Curing temperature is 150 DEG C, and cure time is 2 hours.
Embodiment 1:
In banbury, by 800g CSM, ethylene propylene diene rubber 200g, 50g's
H-501 closes refining 10 minutes under the conditions of 125 DEG C, parks 72 hours after discharge under room temperature;By premixing glue again
Secondary input banbury pressing 2 minutes, add 150g magnesium oxide, 30g stearic acid, 500g white carbon black and
Mixing 8 minutes of 150g poly-suberic acid dibutyl ester, dump temperature controls, between 110-120 DEG C, to park 24
More than hour, addition 80g vulcanizing agent is mixing uniformly on a mill until, thin logical 3 times of 0.5mm roll spacing, 4mm
Roll spacing bottom sheet cools down.Its vulcanization parameters is first cure temperature 170 DEG C, and cure time is 15 points
Clock;Second segment curing temperature is 150 DEG C, and cure time is 2 hours.
Embodiment 2:
In banbury, by 900g CSM, ethylene propylene diene rubber 100g, 50g's
H-501 closes refining 10 minutes under the conditions of 125 DEG C, parks 72 hours after discharge under room temperature;By premixing glue again
Secondary input banbury pressing 2 minutes, add 150g magnesium oxide, 30g stearic acid, 500g white carbon black and
Mixing 8 minutes of 150g poly-suberic acid dibutyl ester, dump temperature controls, between 110-120 DEG C, to park 24
More than hour, addition 80g vulcanizing agent is mixing uniformly on a mill until, thin logical 3 times of 0.5mm roll spacing, 4mm
Roll spacing bottom sheet cools down.Its vulcanization parameters is first cure temperature 170 DEG C, and cure time is 15 points
Clock;Second segment curing temperature is 150 DEG C, and cure time is 2 hours.
Embodiment 3:
In banbury, by 900g CSM, ethylene propylene diene rubber 100g, 30g's
H-501 closes refining 10 minutes under the conditions of 125 DEG C, parks 72 hours after discharge under room temperature;By premixing glue again
Secondary input banbury pressing 2 minutes, add 150g magnesium oxide, 30g stearic acid, 500g white carbon black and
Mixing 8 minutes of 150g poly-suberic acid dibutyl ester, dump temperature controls, between 110-120 DEG C, to park 24
More than hour, addition 80g vulcanizing agent is mixing uniformly on a mill until, thin logical 3 times of 0.5mm roll spacing, 4mm
Roll spacing bottom sheet cools down.Its vulcanization parameters is first cure temperature 170 DEG C, and cure time is 15 points
Clock;Second segment curing temperature is 150 DEG C, and cure time is 2 hours.
Embodiment 4:
In banbury, by 700g CSM, ethylene propylene diene rubber 300g, 30g's
H-501 closes refining 10 minutes under the conditions of 125 DEG C, parks 72 hours after discharge under room temperature;By premixing glue again
Secondary input banbury pressing 2 minutes, add 150g magnesium oxide, 30g stearic acid, 500g white carbon black and
Mixing 8 minutes of 150g poly-suberic acid dibutyl ester, dump temperature controls, between 110-120 DEG C, to park 24
Hour, addition 80g vulcanizing agent is mixing uniformly on a mill until, thin logical 3 times of 0.5mm roll spacing, 4mm roll spacing
Bottom sheet cools down.Its vulcanization parameters is first cure temperature 170 DEG C, and cure time is 15 minutes;
Second segment curing temperature is 150 DEG C, and cure time is 2 hours.
Embodiment 5:
In banbury, by 700g CSM, ethylene propylene diene rubber 300g, 60g's
H-501 closes refining 10 minutes under the conditions of 125 DEG C, parks 72 hours after discharge under room temperature;By premixing glue again
Secondary input banbury pressing 2 minutes, add 150g magnesium oxide, 30g stearic acid, 500g white carbon black and
Mixing 8 minutes of 150g poly-suberic acid dibutyl ester, dump temperature controls, between 110-120 DEG C, to park 72
Hour, addition 80g vulcanizing agent is mixing uniformly on a mill until, thin logical 3 times of 0.5mm roll spacing, 4mm roll spacing
Bottom sheet cools down.Its vulcanization parameters is first cure temperature 170 DEG C, and cure time is 15 minutes;
Second segment curing temperature is 150 DEG C, and cure time is 2 hours.
Embodiment 6:
In banbury, by 700g CSM, ethylene propylene diene rubber 300g, 60g's
H-501 closes refining 10 minutes under the conditions of 125 DEG C, parks 72 hours after discharge under room temperature;By premixing glue again
Secondary input banbury pressing 2 minutes, add 150g magnesium oxide, 30g calcium stearate, 500g white carbon black and
Mixing 8 minutes of 150g poly-adipic acid fourth diester, dump temperature controls, between 110-120 DEG C, to park 24
More than hour, addition 80g vulcanizing agent is mixing uniformly on a mill until, thin logical 3 times of 0.5mm roll spacing, 4mm
Roll spacing bottom sheet cools down.Its vulcanization parameters is first cure temperature 170 DEG C, and cure time is 15 points
Clock;Second segment curing temperature is 150 DEG C, and cure time is 2 hours.
Embodiment 7:
In banbury, by 700g CSM, ethylene propylene diene rubber 300g, 60g's
H-501 closes refining 10 minutes under the conditions of 125 DEG C, parks 72 hours after discharge under room temperature;By premixing glue again
Secondary input banbury pressing 2 minutes, adds 150g magnesium oxide, 15g calcium stearate, 15g N, N '-second
Support bis-stearamides, 600g white carbon black and mixing 8 minutes of 150g poly-adipic acid fourth diester, dump temperature control
System, between 110-120 DEG C, is parked more than 24 hours, is added 80g vulcanizing agent on a mill until uniformly,
Thin logical 3 times of 0.5mm roll spacing, 4mm roll spacing bottom sheet cools down.Its vulcanization parameters is first cure temperature
170 DEG C, cure time is 15 minutes;Second segment curing temperature is 150 DEG C, and cure time is 2 hours.
Embodiment 8:
In banbury, by 700g CSM, ethylene propylene diene rubber 300g, 60g's
H-501 closes refining 10 minutes under the conditions of 125 DEG C, parks 72 hours after discharge under room temperature;By premixing glue again
Secondary input banbury pressing 2 minutes, adds 150g magnesium oxide, 15g calcium stearate, 15g N, N '-second
Support bis-stearamides, 400g white carbon black and mixing 8 minutes of 100g poly-adipic acid fourth diester, dump temperature control
System, between 110-120 DEG C, is parked more than 24 hours, is added 100g vulcanizing agent on a mill until mixing all
Even, thin logical 3 times of 0.5mm roll spacing, 4mm roll spacing bottom sheet cools down.Its vulcanization parameters is first cure
Temperature 170 DEG C, cure time is 15 minutes;Second segment curing temperature is 150 DEG C, and cure time is 2 little
Time.
Embodiment 9:
In banbury, by 700g CSM, ethylene propylene diene rubber 300g, 60g's
H-501 closes refining 10 minutes under the conditions of 125 DEG C, parks 72 hours after discharge under room temperature;By premixing glue again
Secondary input banbury pressing 2 minutes, addition 150g magnesium oxide, 10g calcium stearate, 20g synthesize neatly
Stone, 600g barium sulfate and mixing 8 minutes of 150g poly-adipic acid fourth diester, dump temperature controls
Between 110-120 DEG C, parking more than 24 hours, addition 60g vulcanizing agent is mixing uniformly on a mill until,
Thin logical 3 times of 0.5mm roll spacing, 4mm roll spacing bottom sheet cools down.Its vulcanization parameters is first cure temperature
170 DEG C, cure time is 15 minutes;Second segment curing temperature is 150 DEG C, and cure time is 2 hours.
Embodiment 10:
In banbury, by 700g CSM, ethylene propylene diene rubber 300g, 60g's
H-501 closes refining 10 minutes under the conditions of 125 DEG C, parks 72 hours after discharge under room temperature;By premixing glue again
Secondary input banbury pressing 2 minutes, addition 150g magnesium oxide, 10g calcium stearate, 20g synthesize neatly
Stone, 600g barium sulfate and mixing 8 minutes of 150g poly-adipic acid fourth diester, dump temperature controls
Between 110-120 DEG C, parking more than 24 hours, addition 70g vulcanizing agent is mixing uniformly on a mill until,
Thin logical 3 times of 0.5mm roll spacing, 4mm roll spacing bottom sheet cools down.Its vulcanization parameters is first cure temperature
170 DEG C, cure time is 15 minutes;Second segment curing temperature is 150 DEG C, and cure time is 2 hours.
Embodiment 11:
In banbury, by 700g CSM, ethylene propylene diene rubber 300g, 60g's
H-501 closes refining 8 minutes under the conditions of 130 DEG C, parks 72 hours after discharge under room temperature;By premixing glue again
Secondary input banbury pressing 2 minutes, addition 150g zinc oxide, 10g calcium stearate, 20g synthesize neatly
Stone, 600g barium sulfate and mixing 6 minutes of 150g poly-adipic acid fourth diester, dump temperature controls
Between 110-120 DEG C, parking more than 24 hours, addition 70g vulcanizing agent is mixing uniformly on a mill until,
Thin logical 3 times of 0.5mm roll spacing, 4mm roll spacing bottom sheet cools down.Its vulcanization parameters is first cure temperature
170 DEG C, cure time is 15 minutes;Second segment curing temperature is 150 DEG C, and cure time is 2 hours.
The rubber composite obtaining above-mentioned comparative example and embodiment detects.
Method of testing illustrates: tensile property test is according to GB/T 528-2009 vulcanite or thermoplasticity
The mensuration of rubber tensile ess-strain performance;
According to GB/T 531.1-2008 sulfur during the hardness test of rubber composite
Change rubber or thermoplastic elastomer penetration hardness test method part 1: shore hardness
Meter method (Shao Er hardness);
The compression set test of rubber composite is according to GB/T 7759-1996
Under vulcanite, thermoplastic elastomer room temperature, high temperature and low temperature, compression set measures.
Following table is the result of test:
As can be seen from the above table, the performance of the embodiment test of application technical solution of the present invention is relative to contrast
Example, the physical and mechanical properties of elastomeric material has and the most significantly improves, at a temperature of 150 DEG C high temperature compressed forever
Property deformation significantly reduce.The rubber composite that the present invention obtains has the compression performance of excellence.
Should be understood that these embodiments are merely to illustrate the present invention rather than limit the scope of the present invention.
In addition, it is to be understood that after having read the content that the present invention lectures, those skilled in the art can be to this
Bright making various changes or modifications, these equivalent form of values fall within the application appended claims equally and are limited
Scope.
Claims (10)
1. one kind low buckling chlorosulfonation rubber composite, it is characterised in that include mass parts
Number under each component: CSM 70-90 part, ethylene propylene diene rubber 10-30 part,
Homogeneous agent 3-6 part, activating agent 10-20 part, processing aid 2-5 part, reinforcing agent 40-60 part,
Plasticizer 10-20 part, vulcanizing agent 6-10 part.
Low buckling chlorosulfonation rubber composite the most according to claim 1, its feature
It is: the Mooney viscosity ML of described CSM1+4Control under 100 DEG C of test conditions
Between 50-60, its chlorine mass content is 35%;And the mass content of described ethylene propylene diene rubber is
7-8%.
Low buckling chlorosulfonation rubber composite the most according to claim 1, its feature
It is: described homogeneous agent is anime mixture.
Low buckling chlorosulfonation rubber composite the most according to claim 1, its feature
Being: described activating agent is extra light calcined magnesia, its iodine number is more than 150.
Low buckling chlorosulfonation rubber composite the most according to claim 1, its feature
It is: described processing aid is halogen-absorber and fatty acid and the mixture of derivant thereof,
And the ratio of described halogen-absorber and fatty acid and derivant thereof is 0: 1-1: 0.
Low buckling chlorosulfonation rubber composite the most according to claim 5, its feature
It is: described halogen-absorber is zinc stearate, magnesium stearate, calcium stearate, synthetic hydrotalcite
One of;Described fatty acid and derivant thereof are stearic acid, stearic amide, N, and N '-ethylene is double hard
One of matter amide.
Low buckling chlorosulfonation rubber composite the most according to claim 1, its feature
It is: described reinforcing agent is any one or both in middle particle ardent method white carbon black or modified barium sulphate
Mixture, and the mesh number of described modified barium sulphate is more than 4000 mesh.
Low buckling chlorosulfonation rubber composite the most according to claim 1, its feature
Be: described plasticizer is polyesters plasticizer, and described plasticizer be polyadipate fourth diester,
One of poly-suberic acid dibutyl ester or its complex.
Low buckling chlorosulfonation rubber composite the most according to claim 1, its feature
It is: described vulcanizing agent is peroxide initiator and maleimide paralled system, and wherein institute
State the mass fraction of maleimide no less than 1.5 parts;Described peroxide initiator is peroxidating
Thing diisopropylbenzene (DIPB).
10. a low buckling chlorosulfonation rubber as claimed in any one of claims 1-9 wherein is multiple
The preparation method of condensation material, it is characterised in that comprise the steps:
①「Employing banbury is processed, first by CSM, ethylene propylene diene rubber
And homogeneously refining 8-10 minute is closed in agent under the conditions of 120-130 DEG C, stops after discharge under room temperature
Put 72 hours;
②「Premixing glue is put into again banbury pressing 2 minutes, adds activating agent, process and help
Mixing 6-8 minute of agent, reinforcing agent and plasticizer, dump temperature controls at 110-120
Between DEG C, park more than 24 hours;
③「Add vulcanizing agent on a mill until mixing uniformly, thin logical 3 times of 0.5mm roll spacing, 4mm
Roll spacing bottom sheet cools down;
④「Sulfuration, its vulcanization parameters is first cure temperature 170 DEG C, cure time
It it is 15 minutes;Second segment curing temperature is 150 DEG C, and cure time is 2 hours.
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Cited By (1)
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CN108794909A (en) * | 2018-07-03 | 2018-11-13 | 安徽菲扬新材料有限公司 | A kind of building curtain wall sealing joint strip |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN108794909A (en) * | 2018-07-03 | 2018-11-13 | 安徽菲扬新材料有限公司 | A kind of building curtain wall sealing joint strip |
CN108794909B (en) * | 2018-07-03 | 2021-01-22 | 佛山周信密封条制品有限公司 | Sealing rubber strip for building curtain wall |
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