CN106543692A - A kind of polyurethane elastomer being modified based on sulfur tetrafluoride and preparation method thereof - Google Patents
A kind of polyurethane elastomer being modified based on sulfur tetrafluoride and preparation method thereof Download PDFInfo
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- CN106543692A CN106543692A CN201610961538.8A CN201610961538A CN106543692A CN 106543692 A CN106543692 A CN 106543692A CN 201610961538 A CN201610961538 A CN 201610961538A CN 106543692 A CN106543692 A CN 106543692A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a kind of polyurethane elastomer being modified based on sulfur tetrafluoride and preparation method thereof, is made up of following components proportioning by weight：21～43 parts of polyurethane, 16～39 parts of acrylate, 12～26 parts of isocyanates, 12～25 parts of hexafluorobutyl acrylate, 7～18 parts of sulfur tetrafluoride, 4～11 parts of hexafluoro propanol, 7～18 parts of carborundum, 6～14 parts of magnesium oxide, 7～18 parts of montmorillonite, 5～12 parts of Pulvis Talci.(1) the polyurethane elastomer Oil repellent being modified based on sulfur tetrafluoride of the present invention is increased, and is increased with the contact angle of water, and surface tension is reduced；(2) polyurethane elastomer heat stability of the present invention is improved, with excellent water-fast solvent resistance；(3) polyurethane elastomer maintains preferable hardness, breaking strength, percentage elongation, storage moduluss and surface property.
Description
Technical field
The invention belongs to technical field of material chemistry, is related to a kind of thermoplastic elastomer (TPE), more particularly to it is a kind of based on sulfur tetrafluoride
Modified polyurethane elastomer and preparation method thereof.
Background technology
Polyurethane elastomer has excellent combination property.For general material, consistency and elasticity is often not
Can take into account simultaneously, often attend to one thing and lose sight of another, and polyurethane elastomer hardness range is wide, can accomplish that (Shao Er A types are hard from 10 degree
Degree) to 75 degree (Shao Er D type hardness testers), and common rubber hardness scope is 60 degree to 100 degree of Shao Er A type hardness testers.It is significant
It is that polyurethane elastomer can also keep higher elasticity, percentage elongation to reach 800% within the scope of so wide temperature unexpectedly, very
To higher, and its maximum hardness is 70 degree or so of Shao A type hardness testers during natural rubber percentage elongation 550%.Polyoxy ester elastomer is general
Not filled and plasticizer, its elasticity can be adjusted by formula；The size of polyurethane elastomer hardness depends on expanding
The structure and molecular weight of the type and consumption of chain agent, the type and consumption of diisocyanate and polyester (ether) polyhydric alcohol.
Another most important characteristic of polyurethane elastomer is that, with high-wearing feature, laboratory measures polyurethane elastomer
Wearability be 3～5 times of natural rubber, and tend to up to more than 10 times in actual applications, therefore, polyurethane elastomer
Have the title of " abrasive rubber ".If adding molybdenum bisuphide, graphite or cassia oil wherein, moreover it is possible to further improve its wear-resisting journey
Degree.Additionally, polyurethane elastomer also has other various features, such as：Load support capacity is big, compared with other rubber, using when
Material can be saved；Good damping effect, endurance shock resistance；Oil resistance is better than nitrile rubber, and anti-weather-aging property is better than day
Right rubber and other synthetic rubber etc..In a word, polyurethane possesses excellent properties, it has both plastics and rubber is numerous valuable
Characteristic, compared with plastics, not embrittlement, wear-resisting；Compared with traditional rubber, wear-resisting, tear-resistant, high-mechanic, intensity are high, hardness range
Extensively.
In marine oil and gas exploitation, polyurethane material can be adopted to make the pipeline of On The Oil And Gas Transportation, this pipeline strength is high,
Corrosion-resistant, life-span length, through fibre-reinforced thermoplastic composite flexible pipe, is particularly well-suited to the high voltage tolerant input trachea of diving operation
With the high voltage tolerant input oil pipe on military hardware.In addition, halogen-free anti-inflaming polyurethane CABLE MATERIALS also skyscraper, tunnel, nuclear power station,
Increasingly extensive use in the special occasions such as seabed engineering.In a word, with the high speed development of Chinese national economy, to elastic polyurethane
The range of application of body will be increasingly wider, and consumption is increasing, and the requirement to performance also will more and more higher.But polyurethane is thin
Water poor-performing, by blending and the method for chemical reaction in prior art, fluorine element is incorporated in polyurethane, but traditional
Fluorine-containing acrylate and the direct physical blending of polyurethane are obtained into the method less use now of fluorochemical urethane.And the method
The surface property of polyurethane can be affected.
The content of the invention
The purpose of the present invention is：In order to overcome the defect of prior art, a kind of hydrophobic performance of acquisition is good, and ensures its surface
The polyurethane elastomer of performance, the invention provides a kind of polyurethane elastomer being modified based on sulfur tetrafluoride and its preparation side
Method.
Technical scheme：A kind of polyurethane elastomer being modified based on sulfur tetrafluoride, by following components proportioning by weight
Make：21～43 parts of polyurethane, 16～39 parts of acrylate, 12～26 parts of isocyanates, 12～25 parts of hexafluorobutyl acrylate,
7～18 parts of sulfur tetrafluoride, 4～11 parts of hexafluoro propanol, 7～18 parts of carborundum, 6～14 parts of magnesium oxide, 7～18 parts of montmorillonite, cunning
5～12 parts of stone powder.
Preferably, it is made up of following components proportioning by weight：36 parts of polyurethane, 32 parts of acrylate, isocyanates
21 parts, 20 parts of hexafluorobutyl acrylate, 12 parts of sulfur tetrafluoride, 8 parts of hexafluoro propanol, 12 parts of carborundum, 11 parts of magnesium oxide, montmorillonite
13 parts, 8 parts of Pulvis Talci.
A kind of method for preparing polyurethane elastic body being modified based on sulfur tetrafluoride, is comprised the steps of：
(1) prepared by matrix：Polyurethane and acrylate are mixed, in adding banbury, blending temperature is 112～145 DEG C,
The blending time is 8～23 minutes, and blending is placed 8～14 hours after terminating under the conditions of 95～130 DEG C；Add stabilizer and plasticising
Agent continues blending 9～22 minutes under the conditions of 110～140 DEG C, obtains final product matrix；
(2) prepared by modifying agent：Sulfur tetrafluoride, hexafluoro propanol, carborundum, magnesium oxide, montmorillonite and Pulvis Talci are mixed, is ground
Grinds, powder diameter are 50～100 mesh；It is placed in electric furnace, heats 1～3.5 hour under the conditions of 115～140 DEG C；
(3) modified blending for the first time：In the matrix for adding step (1) to obtain modifying agent obtained in step (2), 105～
130 DEG C knead 9～21 minutes, are placed 6～12 hours after terminating under the conditions of 96～116 DEG C；
(4) primary vulcanization：Vulcanizing agent is added in the raw material after the modified blending of step (3), after stirring 100～
Place 5～15 hours under the conditions of 125 DEG C；
(5) second modified blending：Isocyanates, hexafluorobutyl acrylate and sulfur tetrafluoride are added into Jing primary vulcanizations
In material afterwards, 105～135 DEG C knead 8～22 minutes；
(6) vulcanize for second：Vulcanizing agent is added in the material Jing after second modified blending of step (5), is stirred
Place 6～15 hours under the conditions of 102～137 DEG C afterwards；
(7) prepared by elastomer：The product of step (6) is placed in mill, masterbatch is refined under the conditions of 115～140 DEG C
System is transparent, you can be obtained.
Preferably, prepared by step (1) matrix：Polyurethane and acrylate are mixed, in adding banbury, blending temperature is
135 DEG C, the blending time is 18 minutes, and blending is placed 11 hours after terminating under the conditions of 122 DEG C；Stabilizer and plasticizer is added to exist
Continue blending 18 minutes under the conditions of 128 DEG C, obtain final product matrix.
Preferably, prepared by step (2) modifying agent：By sulfur tetrafluoride, hexafluoro propanol, carborundum, magnesium oxide, montmorillonite and cunning
Stone powder is mixed, and is pulverized, and powder diameter is 70 mesh；It is placed in electric furnace, heats 2.5 hours under the conditions of 129 DEG C.
Preferably, step (3) modified blending for the first time：The base that modifying agent addition step (1) obtained in step (2) is obtained
In body, 122 DEG C knead 16 minutes, are placed 9 hours after terminating under the conditions of 105 DEG C.
Preferably, step (4) primary vulcanization：Vulcanizing agent is added in the raw material after the modified blending of step (3), stirring is equal
Place 12 hours under the conditions of 118 DEG C after even.
Preferably, second modified blending of step (5)：Isocyanates, hexafluorobutyl acrylate and sulfur tetrafluoride are added
In material Jing after primary vulcanization, 126 DEG C knead 18 minutes.
Preferably, step (6) vulcanizes for second：Sulfuration is added in the material Jing after second modified blending of step (5)
Agent, places 13 hours after stirring under the conditions of 128 DEG C.
Preferably, prepared by step (7) elastomer：The product of step (6) is placed in mill, will under the conditions of 134 DEG C
Masterbatch refining is transparent, you can be obtained.
Beneficial effect：(1) the polyurethane elastomer Oil repellent being modified based on sulfur tetrafluoride of the present invention is increased, with water
Contact angle increases, and surface tension is reduced；(2) polyurethane elastomer heat stability of the present invention is improved, with excellent water-fast
Solvent resistance；(3) polyurethane elastomer maintains preferable hardness, breaking strength, percentage elongation, storage moduluss and surface
Performance.
Specific embodiment
Embodiment 1
A kind of polyurethane elastomer being modified based on sulfur tetrafluoride, is made up of following components proportioning by weight：Poly- ammonia
21 parts of ester, 16 parts of acrylate, 12 parts of isocyanates, 12 parts of hexafluorobutyl acrylate, 7 parts of sulfur tetrafluoride, 4 parts of hexafluoro propanol,
7 parts of carborundum, 6 parts of magnesium oxide, 7 parts of montmorillonite, 5 parts of Pulvis Talci.
A kind of method for preparing polyurethane elastic body being modified based on sulfur tetrafluoride, is comprised the steps of：
(1) prepared by matrix：Polyurethane and acrylate are mixed, in adding banbury, blending temperature is 112 DEG C, blending
Time is 8 minutes, and blending is placed 8 hours after terminating under the conditions of 95 DEG C；Add stabilizer and plasticizer under the conditions of 110 DEG C after
Continuous blending 9 minutes, obtains final product matrix；
(2) prepared by modifying agent：Sulfur tetrafluoride, hexafluoro propanol, carborundum, magnesium oxide, montmorillonite and Pulvis Talci are mixed, is ground
Grinds, powder diameter are 50 mesh；It is placed in electric furnace, heats 1 hour under the conditions of 115 DEG C；
(3) modified blending for the first time：In the matrix for adding step (1) to obtain modifying agent obtained in step (2), 105 DEG C
Mixing 9 minutes, places 6 hours after terminating under the conditions of 96 DEG C；
(4) primary vulcanization：Vulcanizing agent is added in the raw material after the modified blending of step (3), at 100 DEG C after stirring
Under the conditions of place 5 hours；
(5) second modified blending：Isocyanates, hexafluorobutyl acrylate and sulfur tetrafluoride are added into Jing primary vulcanizations
In material afterwards, 105 DEG C knead 8 minutes；
(6) vulcanize for second：Vulcanizing agent is added in the material Jing after second modified blending of step (5), is stirred
Place 6 hours under the conditions of 102 DEG C afterwards；
(7) prepared by elastomer：The product of step (6) is placed in mill, will be masterbatch refining saturating under the conditions of 115 DEG C
It is bright, you can be obtained.
Embodiment 2
A kind of polyurethane elastomer being modified based on sulfur tetrafluoride, is made up of following components proportioning by weight：Poly- ammonia
36 parts of ester, 32 parts of acrylate, 21 parts of isocyanates, 20 parts of hexafluorobutyl acrylate, 12 parts of sulfur tetrafluoride, 8 parts of hexafluoro propanol,
12 parts of carborundum, 11 parts of magnesium oxide, 13 parts of montmorillonite, 8 parts of Pulvis Talci.
A kind of method for preparing polyurethane elastic body being modified based on sulfur tetrafluoride, is comprised the steps of：
(1) prepared by matrix：Polyurethane and acrylate are mixed, in adding banbury, blending temperature is 135 DEG C, blending
Time is 18 minutes, and blending is placed 11 hours after terminating under the conditions of 122 DEG C；Stabilizer and plasticizer are added in 128 DEG C of conditions
It is lower to continue blending 18 minutes, obtain final product matrix；
(2) prepared by modifying agent：Sulfur tetrafluoride, hexafluoro propanol, carborundum, magnesium oxide, montmorillonite and Pulvis Talci are mixed, is ground
Grinds, powder diameter are 70 mesh；It is placed in electric furnace, heats 2.5 hours under the conditions of 129 DEG C；
(3) modified blending for the first time：In the matrix for adding step (1) to obtain modifying agent obtained in step (2), 122 DEG C
Mixing 16 minutes, places 9 hours after terminating under the conditions of 105 DEG C；
(4) primary vulcanization：Vulcanizing agent is added in the raw material after the modified blending of step (3), at 118 DEG C after stirring
Under the conditions of place 12 hours；
(5) second modified blending：Isocyanates, hexafluorobutyl acrylate and sulfur tetrafluoride are added into Jing primary vulcanizations
In material afterwards, 126 DEG C knead 18 minutes；
(6) vulcanize for second：Vulcanizing agent is added in the material Jing after second modified blending of step (5), is stirred
Place 13 hours under the conditions of 128 DEG C afterwards；
(7) prepared by elastomer：The product of step (6) is placed in mill, will be masterbatch refining saturating under the conditions of 134 DEG C
It is bright, you can be obtained.
Embodiment 3
A kind of polyurethane elastomer being modified based on sulfur tetrafluoride, is made up of following components proportioning by weight：Poly- ammonia
43 parts of ester, 39 parts of acrylate, 26 parts of isocyanates, 25 parts of hexafluorobutyl acrylate, 18 parts of sulfur tetrafluoride, hexafluoro propanol 11
Part, 18 parts of carborundum, 14 parts of magnesium oxide, 18 parts of montmorillonite, 12 parts of Pulvis Talci.
A kind of method for preparing polyurethane elastic body being modified based on sulfur tetrafluoride, is comprised the steps of：
(1) prepared by matrix：Polyurethane and acrylate are mixed, in adding banbury, blending temperature is 145 DEG C, blending
Time is 23 minutes, and blending is placed 14 hours after terminating under the conditions of 130 DEG C；Stabilizer and plasticizer are added in 140 DEG C of conditions
It is lower to continue blending 22 minutes, obtain final product matrix；
(2) prepared by modifying agent：Sulfur tetrafluoride, hexafluoro propanol, carborundum, magnesium oxide, montmorillonite and Pulvis Talci are mixed, is ground
Grinds, powder diameter are 100 mesh；It is placed in electric furnace, heats 3.5 hours under the conditions of 140 DEG C；
(3) modified blending for the first time：In the matrix for adding step (1) to obtain modifying agent obtained in step (2), 130 DEG C
Mixing 21 minutes, places 12 hours after terminating under the conditions of 116 DEG C；
(4) primary vulcanization：Vulcanizing agent is added in the raw material after the modified blending of step (3), at 125 DEG C after stirring
Under the conditions of place 15 hours；
(5) second modified blending：Isocyanates, hexafluorobutyl acrylate and sulfur tetrafluoride are added into Jing primary vulcanizations
In material afterwards, 135 DEG C knead 22 minutes；
(6) vulcanize for second：Vulcanizing agent is added in the material Jing after second modified blending of step (5), is stirred
Place 15 hours under the conditions of 137 DEG C afterwards；
(7) prepared by elastomer：The product of step (6) is placed in mill, will be masterbatch refining saturating under the conditions of 140 DEG C
It is bright, you can be obtained.
The polyurethane elastomer being modified based on sulfur tetrafluoride prepared to embodiment 1～3 is detected, as a result as follows
Shown in table：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Breaking strength/MPa | 22.3 | 27.7 | 25.8 |
| Tearing strength/KN/M | 91 | 112 | 106 |
| Elongation at break/% | 845 | 875 | 863 |
| Limited oxygen index | 11 | 6 | 9 |
| Surface energy/mN/m | 34.2 | 31.2 | 32.4 |
| Contact angle/° | 94.3 | 91.5 | 92.7 |
Claims (10)
1. it is a kind of based on sulfur tetrafluoride be modified polyurethane elastomer, it is characterised in that by following components proportioning by weight
Make：21～43 parts of polyurethane, 16～39 parts of acrylate, 12～26 parts of isocyanates, 12～25 parts of hexafluorobutyl acrylate,
7～18 parts of sulfur tetrafluoride, 4～11 parts of hexafluoro propanol, 7～18 parts of carborundum, 6～14 parts of magnesium oxide, 7～18 parts of montmorillonite, cunning
5～12 parts of stone powder.
2. it is according to claim 1 it is a kind of based on sulfur tetrafluoride be modified polyurethane elastomer, it is characterised in that by following
Component proportioning by weight is made：36 parts of polyurethane, 32 parts of acrylate, 21 parts of isocyanates, hexafluorobutyl acrylate 20
Part, 12 parts of sulfur tetrafluoride, 8 parts of hexafluoro propanol, 12 parts of carborundum, 11 parts of magnesium oxide, 13 parts of montmorillonite, 8 parts of Pulvis Talci.
3. described in claim 1 it is a kind of based on sulfur tetrafluoride be modified method for preparing polyurethane elastic body, it is characterised in that
Comprise the steps of：
(1) prepared by matrix：Polyurethane and acrylate are mixed, in adding banbury, blending temperature is 112～145 DEG C, blending
Time is 8～23 minutes, and blending is placed 8～14 hours after terminating under the conditions of 95～130 DEG C；Stabilizer and plasticizer is added to exist
Continue blending 9～22 minutes under the conditions of 110～140 DEG C, obtain final product matrix；
(2) prepared by modifying agent：Sulfur tetrafluoride, hexafluoro propanol, carborundum, magnesium oxide, montmorillonite and Pulvis Talci are mixed, is ground to form
Powder, powder diameter are 50～100 mesh；It is placed in electric furnace, heats 1～3.5 hour under the conditions of 115～140 DEG C；
(3) modified blending for the first time：In the matrix for adding step (1) to obtain modifying agent obtained in step (2), 105～130 DEG C
Mixing 9～21 minutes, places 6～12 hours after terminating under the conditions of 96～116 DEG C；
(4) primary vulcanization：Vulcanizing agent is added in the raw material after the modified blending of step (3), 100～125 after stirring
Place 5～15 hours under the conditions of DEG C；
(5) second modified blending：Isocyanates, hexafluorobutyl acrylate and sulfur tetrafluoride are added Jing after primary vulcanization
In material, 105～135 DEG C knead 8～22 minutes；
(6) vulcanize for second：Vulcanizing agent is added in the material Jing after second modified blending of step (5), after stirring
Place 6～15 hours under the conditions of 102～137 DEG C；
(7) prepared by elastomer：The product of step (6) is placed in mill, will be masterbatch refining saturating under the conditions of 115～140 DEG C
It is bright, you can be obtained.
4. it is according to claim 3 it is a kind of based on sulfur tetrafluoride be modified method for preparing polyurethane elastic body, its feature
It is prepared by step (1) matrix：Polyurethane and acrylate are mixed, in adding banbury, blending temperature is 135 DEG C, blending
Time is 18 minutes, and blending is placed 11 hours after terminating under the conditions of 122 DEG C；Stabilizer and plasticizer are added in 128 DEG C of conditions
It is lower to continue blending 18 minutes, obtain final product matrix.
5. it is according to claim 3 it is a kind of based on sulfur tetrafluoride be modified method for preparing polyurethane elastic body, its feature
It is prepared by step (2) modifying agent：Sulfur tetrafluoride, hexafluoro propanol, carborundum, magnesium oxide, montmorillonite and Pulvis Talci are mixed,
Pulverize, powder diameter is 70 mesh；It is placed in electric furnace, heats 2.5 hours under the conditions of 129 DEG C.
6. it is according to claim 3 it is a kind of based on sulfur tetrafluoride be modified method for preparing polyurethane elastic body, its feature
It is, step (3) modified blending for the first time：In the matrix for adding step (1) to obtain modifying agent obtained in step (2), 122 DEG C
Mixing 16 minutes, places 9 hours after terminating under the conditions of 105 DEG C.
7. it is according to claim 3 it is a kind of based on sulfur tetrafluoride be modified method for preparing polyurethane elastic body, its feature
It is, step (4) primary vulcanization：Vulcanizing agent is added in the raw material after the modified blending of step (3), 118 after stirring
Place 12 hours under the conditions of DEG C.
8. it is according to claim 3 it is a kind of based on sulfur tetrafluoride be modified method for preparing polyurethane elastic body, its feature
It is, second modified blending of step (5)：Isocyanates, hexafluorobutyl acrylate and sulfur tetrafluoride are added into Jing first time sulfur
In material after change, 126 DEG C knead 18 minutes.
9. it is according to claim 3 it is a kind of based on sulfur tetrafluoride be modified method for preparing polyurethane elastic body, its feature
It is that step (6) vulcanizes for second：Vulcanizing agent is added in the material Jing after second modified blending of step (5), is stirred
Place 13 hours under the conditions of 128 DEG C afterwards.
10. it is according to claim 3 it is a kind of based on sulfur tetrafluoride be modified method for preparing polyurethane elastic body, its feature
It is prepared by step (7) elastomer：The product of step (6) is placed in mill, will be masterbatch refining saturating under the conditions of 134 DEG C
It is bright, you can be obtained.
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Cited By (3)
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| CN108587113A (en) * | 2018-03-20 | 2018-09-28 | 浙江工业大学 | A kind of preparation method of self-cleaning polyurethane elastomer film |
| CN109575222A (en) * | 2018-12-13 | 2019-04-05 | 江南大学 | A kind of composite modified UV of fluoro- sulphur solidifies the preparation method of multi-arm type aqueous polyurethane |
| CN110938267A (en) * | 2019-12-04 | 2020-03-31 | 安徽国电能源设备工程有限公司 | Preparation method of weather-resistant flame-retardant environment-friendly water heating blanket hose |
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| CN108587113A (en) * | 2018-03-20 | 2018-09-28 | 浙江工业大学 | A kind of preparation method of self-cleaning polyurethane elastomer film |
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| CN109575222A (en) * | 2018-12-13 | 2019-04-05 | 江南大学 | A kind of composite modified UV of fluoro- sulphur solidifies the preparation method of multi-arm type aqueous polyurethane |
| CN110938267A (en) * | 2019-12-04 | 2020-03-31 | 安徽国电能源设备工程有限公司 | Preparation method of weather-resistant flame-retardant environment-friendly water heating blanket hose |
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Application publication date: 20170329 |