CN110330626A - Sealing fire-resistant high-resiliency polyurethane and its processing technology - Google Patents
Sealing fire-resistant high-resiliency polyurethane and its processing technology Download PDFInfo
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- CN110330626A CN110330626A CN201910464126.7A CN201910464126A CN110330626A CN 110330626 A CN110330626 A CN 110330626A CN 201910464126 A CN201910464126 A CN 201910464126A CN 110330626 A CN110330626 A CN 110330626A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6603—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6607—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
- C08G18/6611—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203 having at least three hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
Abstract
The invention discloses a kind of sealing fire-resistant high-resiliency polyurethane, including following parts by weight to form: 30~50 parts of paraphenylene diisocyanate；40~60 parts of polytetrahydrofuran；50~70 parts of polyester polyol；2~5 parts of trimethylolpropane；10~20 parts of 1,4- butanediol；1~3 part of antioxidant；2~4 parts of filler.Paraphenylene diisocyanate type thermo-plastic polyurethane elastomer of the present invention greatly expands the temperature range of polyurethane material application, improves the high temperature resistance of polyurethane material, and improve the stability that polyurethane works at high temperature.
Description
Technical field
The present invention relates to a kind of sealing fire-resistant high-resiliency polyurethane and its processing technology.
Background technique
In the prior art, the sealing element in digging machine master cylinder is made of polyurethane elastomeric materials.Digging machine master cylinder operating condition: 1,
Movement velocity is fast, 1 meter per second.2, pressure is high, 45MPA.3, limiting temperature is high, and frictional heat generation is severe, and maximum operating temperature reaches
115 degree.4, variation of ambient temperature is big, and winter low temperature is to -25 DEG C, and summer high-temperature is to 40 DEG C.
Best polyurethane elastomer material operating temperature heat resistance is no more than 110 DEG C currently on the market, and works as work
When temperature reaches 100 or more, the hot dynamic property of material sharply declines, and material steps into viscous state by elastomeric state, follows the string
The sealing characteristics of body.Therefore the sealing element of existing polyurethane elastomer material production on the market can no longer meet digging machine oil cylinder
Work requirements, therefore there is improved spaces.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of sealing fire-resistant high-resiliency polyurethane and its processing works
Skill has been obviously improved the high temperature resistance of polyurethane and the stability of material.
To achieve the above object, the present invention provides the following technical scheme that
A kind of sealing fire-resistant high-resiliency polyurethane, it is characterized in that: including that following parts by weight form:
30~50 parts of paraphenylene diisocyanate；
40~60 parts of polytetrahydrofuran；
50~70 parts of polyester polyol；
2~5 parts of trimethylolpropane；
10~20 parts of 1,4- butanediol；
1~3 part of antioxidant；
2~4 parts of filler.
Preferably, the antioxidant is made of one or more of antioxidant 245, antioxidant 264 and antioxidant 1330.
Preferably, the filler selects one or more of nanometer materials, superfines of self-lubrication.
A kind of sealing processing technology of fire-resistant high-resiliency polyurethane, it is characterized in that:
40~60 parts of polytetrahydrofuran and 50~70 parts of polyester-diols are added in a kettle, is stirred using low speed by step a
It mixes, temperature of reaction kettle is controlled in 90 degrees centigrades；
Step b is added 1~3 part of antioxidant and 2~4 fillers, using high-speed stirred and vacuumizes, temperature of reaction kettle control
Between 100~110 degrees Celsius；
Step c after 1~2 hour, is added 30~50 parts of paraphenylene diisocyanate, using high-speed stirred and vacuumizes, hold
After continuous reaction 5~8 hours, base polyurethane prepolymer for use as is obtained；
10~20 parts of 1,4-butanediol and 2~5 parts of trimethylolpropanes are first sufficiently mixed, obtain mixed liquor by step d；
Performed polymer is heated to 80~100 DEG C, 10~25 portions of mixed liquors is added, stirs evenly rapidly, pours into pre- by step e
In the mold of heat, vulcanize 15~25 hours in 90~110 DEG C of baking oven, places 6~9 hours, can be prepared by the poly- ammonia of high temperature resistant
Ester elastomer material.
Preferably, in step a, the molecular weight of polytetrahydrofuran is 2000, and the molecular weight of polyester-diol is 2400.
Preferably, in step c, the hydroxyl value of obtained base polyurethane prepolymer for use as is measured, hydroxyl value needs again less than 90%
Reaction, hydroxyl value, which is more than or equal to 90%, can carry out subsequent job.
Preferably, in step d, the moisture in still air enters in mixed liquor.
Advantages of the present invention are as follows: paraphenylene diisocyanate type thermo-plastic polyurethane elastomer greatly expands polyurethanes material
The temperature range for expecting application, improves the high temperature resistance of polyurethane material, and improve what polyurethane worked at high temperature
Stability.
Detailed description of the invention
Fig. 1 is the hot dynamic property comparison diagram of polyurethane material and existing polyurethane material of the invention.
Specific embodiment
A kind of sealing fire-resistant high-resiliency polyurethane, it is characterized in that: including that following parts by weight form:
30~50 parts of paraphenylene diisocyanate；
40~60 parts of polytetrahydrofuran；
50~70 parts of polyester polyol；
2~5 parts of trimethylolpropane；
10~20 parts of 1,4- butanediol；
1~3 part of antioxidant；
2~4 parts of filler.
The selection of antioxidant is one or more of antioxidant 245, antioxidant 264 and antioxidant 1330.
The selection of filler is one or more of nanometer materials, the superfines of self-lubrication.
The processing technology of above-mentioned sealing fire-resistant high-resiliency polyurethane:
40~60 parts of polytetrahydrofuran and 50~70 parts of polyester-diols are added in a kettle, is stirred using low speed by step a
It mixes, temperature of reaction kettle is controlled in 90 degrees centigrades；
Step b is added 1~3 part of antioxidant and 2~4 fillers, using high-speed stirred and vacuumizes, temperature of reaction kettle control
Between 100~110 degrees Celsius；
Step c after 1~2 hour, is added 30~50 parts of paraphenylene diisocyanate, using high-speed stirred and vacuumizes, hold
After continuous reaction 5~8 hours, base polyurethane prepolymer for use as is obtained；
10~20 parts of 1,4-butanediol and 2~5 parts of trimethylolpropanes are first sufficiently mixed, obtain mixed liquor by step d；
Performed polymer is heated to 80~100 DEG C, 10~25 portions of mixed liquors is added, stirs evenly rapidly, pours into pre- by step e
In the mold of heat, vulcanize 15~25 hours in 90~110 DEG C of baking oven, places 6~9 hours, can be prepared by the poly- ammonia of high temperature resistant
Ester elastomer material.
Compared with traditional thermo-plastic polyurethane's material, paraphenylene diisocyanate type thermo-plastic polyurethane's elastomer greatly expands
The temperature range of polyurethane material application.Since paraphenylene diisocyanate molecular machinery is symmetrical, lack steric hindrance pendent group,
Therefore this has splendid hard section chain to stack efficiency diisocyanate and mutually separates with good.It chemically measures than for upper, though
Right paraphenylene diisocyanate and MDI have similar formula, hardness and modulus properties compared with TODI, but to benzene diisocyanate
In ester, isocyanates is lower in the molar ratio of polyalcohol.The trend reflects the lower steric hindrance intrinsic to benzene structure and higher
Stack efficiency.These above-mentioned attributes make high resiliency paraphenylene diisocyanate type thermo-plastic polyurethane material is very applicable to be applied to want
It asks in lowest loss and the industry of high-fire resistance.Test data shows that paraphenylene diisocyanate type thermo-plastic polyurethane's elastomer has
Have unique dynamic property and heat resistance compare for have very big promotion, this will be enlarged by thermo-plastic polyurethane's elastomer in crucial work
Application in journey.So that the heatproof of the polyurethane material is up to 130 degrees Celsius, instantaneous high temperature resistant is at 150 degrees Celsius, therefore
It has been obviously improved high temperature resistance, and has enabled component made of this polyurethane material under 120 degrees Celsius or less operating conditions
Steady operation.
Specific processing technology:
Embodiment 1: polytetrahydrofuran and 52 parts of molecules that 41 parts of molecular weight are 2000 is added in step a in a kettle
The polyester-diol that amount is 2400, is stirred using revolving speed in 100~200 low speed of walking around, and temperature of reaction kettle control is taken the photograph 90
Family name's degree or so；
1 part of combination antioxidant and 2 parts of fillers are added in step b, are stirred simultaneously using revolving speed in 2000 turns or more be carried out at high speed
And will be vacuumized inside stirred tank, temperature of reaction kettle controls between 100~110 degrees Celsius；
After 1~2 hour, 30 parts of paraphenylene diisocyanate are added in step c, and the height using revolving speed at 1500 turns or more turns
Speed continues to stir and vacuumize again, after sustained response 5~8 hours, obtains base polyurethane prepolymer for use as, pre- to obtained polyurethane
The hydroxyl value of aggressiveness measures, and hydroxyl value need to react again less than 90%, and hydroxyl value, which is more than or equal to 90%, can carry out subsequent job；
10 parts of 1,4-butanediol and 2 parts of trimethylolpropanes are first sufficiently mixed, obtain mixed liquor by step d, the mixed liquor
During the preparation process, the moisture in air is forbidden to enter the mixed liquor, because easily causing secondary anti-after moisture enters the mixed liquor
It answers, influences whether the mechanical property of material, and moisture can react generation carbon dioxide in the material, generated in material internal big
Gas is measured, when injection molding can foam, and reduce quality of materials；
Performed polymer is heated to 80~100 DEG C by step e, and 10 portions of mixed liquors are added, stirs evenly rapidly, pours into preheating
In mold, vulcanize 15~25 hours in 90~110 DEG C of baking oven, places 6~9 hours, can be prepared by high temperature resistant polyurethane bullet
Property material.
Embodiment 2: polytetrahydrofuran and 62 parts of molecules that 51 parts of molecular weight are 2000 is added in step a in a kettle
The polyester-diol that amount is 2400, is stirred using revolving speed in 100~200 slow-speed of revolution, and temperature of reaction kettle control is Celsius 90
Degree left and right；
1.2 parts of combination antioxidant and 2 parts of fillers are added in step b, are carried out at high speed stirring at 2000 turns or more using revolving speed
And it will be vacuumized inside stirred tank, temperature of reaction kettle controls between 100~110 degrees Celsius；
After 1~2 hour, 41 parts of paraphenylene diisocyanate are added in step c, and the height using revolving speed at 1500 turns or more turns
Speed continues to stir and vacuumize again, after sustained response 5~8 hours, obtains base polyurethane prepolymer for use as, pre- to obtained polyurethane
The hydroxyl value of aggressiveness measures, and hydroxyl value need to react again less than 90%, and hydroxyl value, which is more than or equal to 90%, can carry out subsequent job；
13 parts of 1,4-butanediol and 3 parts of trimethylolpropanes are first sufficiently mixed, obtain mixed liquor by step d, the mixed liquor
During the preparation process, moisture in air need to be forbidden to enter the mixed liquor, therefore after moisture enters the mixed liquor, easily caused secondary anti-
It answers, influences whether the mechanical property of material, and moisture can react generation carbon dioxide in material, generated in material internal a large amount of
Gas, when injection molding, can foam, and reduce quality of materials；
Performed polymer is heated to 80~100 DEG C by step e, and 10 portions of mixed liquors are added, stirs evenly rapidly, pours into preheating
In mold, vulcanize 15~25 hours in 90~110 DEG C of baking oven, places 6~9 hours, can be prepared by high temperature resistant polyurethane bullet
Property material.
Embodiment 3: polytetrahydrofuran and 66 parts of molecules that 56 parts of molecular weight are 2000 is added in step a in a kettle
The polyester-diol that amount is 2400, is stirred using revolving speed in 100~200 slow-speed of revolution, and temperature of reaction kettle control is Celsius 90
Degree left and right；
1.5 parts of combination antioxidant and 3 parts of fillers are added in step b, are carried out at high speed stirring at 2000 turns or more using revolving speed
And it will be vacuumized inside stirred tank, temperature of reaction kettle controls between 100~110 degrees Celsius；
After 1~2 hour, 49 parts of paraphenylene diisocyanate are added in step c, and the height using revolving speed at 1500 turns or more turns
Speed continues to stir and vacuumize again, after sustained response 5~8 hours, obtains base polyurethane prepolymer for use as, pre- to obtained polyurethane
The hydroxyl value of aggressiveness measures, and hydroxyl value need to react again less than 90%, and hydroxyl value, which is more than or equal to 90%, can carry out subsequent job；
17 parts of 1,4-butanediol and 4 parts of trimethylolpropanes are first sufficiently mixed, obtain mixed liquor by step d, the mixed liquor
During the preparation process, moisture in air need to be forbidden to enter the mixed liquor, therefore after moisture enters the mixed liquor, easily caused secondary anti-
It answers, influences whether the mechanical property of material, and moisture can react generation carbon dioxide in material, generated in material internal a large amount of
Gas, when injection molding, can foam, and reduce quality of materials；
Performed polymer is heated to 80~100 DEG C by step e, and 15 portions of mixed liquors are added, stirs evenly rapidly, pours into preheating
In mold, vulcanize 15~25 hours in 90~110 DEG C of baking oven, places 6~9 hours, can be prepared by high temperature resistant polyurethane bullet
Property material.
In above-mentioned technical process, strictly controlled environment temperature and humidity is needed, the variation of environment leads to the shakiness of material property
It is fixed.
Following table is high temperature resistant high-rebound polyurethane material of the present invention and conventional polyurethanes characteristic of material mechanics contrast table:
Unless otherwise specified, the present invention in, if having term " width ", "upper", "lower", "front", "rear", "left", "right",
The instruction such as "vertical", "horizontal", "top", "bottom" "inner", "outside", " clockwise ", " counterclockwise ", " axial direction ", " radial direction ", " circumferential direction "
Orientation or positional relationship be to be based on the orientation or positional relationship shown in the drawings, be merely for convenience of description the present invention and simplification retouch
It states, rather than the device or element of indication or suggestion meaning must have a particular orientation, be constructed and operated in a specific orientation,
Therefore the term for describing orientation or positional relationship in the present invention only for illustration, should not be understood as the limit to this patent
System, for the ordinary skill in the art, can be in conjunction with attached drawing, and understands the specific of above-mentioned term as the case may be
Meaning.
Unless otherwise clearly defined and limited, in the present invention, if there is term " setting ", " connected " and " connection " that should do extensively
Reason and good sense solution may be a detachable connection for example, it may be being fixedly connected, or be integrally connected；It can be directly connected,
The connection inside two elements can be can be indirectly connected through an intermediary.For those of ordinary skill in the art and
Speech, can understand the concrete meaning of above-mentioned term in the present invention with concrete condition.
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-mentioned implementation
Example, all technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
Those of ordinary skill for, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (7)
1. a kind of sealing fire-resistant high-resiliency polyurethane, it is characterized in that: including that following parts by weight form:
30~50 parts of paraphenylene diisocyanate；
40~60 parts of polytetrahydrofuran；
50~70 parts of polyester polyol；
2~5 parts of trimethylolpropane；
10~20 parts of 1,4- butanediol；
1~3 part of antioxidant；
2~4 parts of filler.
2. sealing fire-resistant high-resiliency polyurethane according to claim 1, it is characterized in that: the antioxidant is by antioxidant
245, one or more of antioxidant 264 and antioxidant 1330 form.
3. sealing fire-resistant high-resiliency polyurethane according to claim 1, it is characterized in that: the filler selects nanoscale
One or more of material, superfines of self-lubrication.
4. a kind of sealing processing technology of fire-resistant high-resiliency polyurethane, it is characterized in that:
40~60 parts of polytetrahydrofuran and 50~70 parts of polyester-diols is added in step a in a kettle, using stirring at low speed,
Temperature of reaction kettle is controlled in 90 degrees centigrades；
Step b is added 1~3 part of antioxidant and 2~4 fillers, using high-speed stirred and vacuumizes, and temperature of reaction kettle is controlled 100
Between~110 degrees Celsius；
Step c after 1~2 hour, is added 30~50 parts of paraphenylene diisocyanate, using high-speed stirred and vacuumizes, and continues anti-
After answering 5~8 hours, base polyurethane prepolymer for use as is obtained；
10~20 parts of 1,4-butanediol and 2~5 parts of trimethylolpropanes are first sufficiently mixed, obtain mixed liquor by step d；
Performed polymer is heated to 80~100 DEG C, 10~25 portions of mixed liquors is added, stirs evenly rapidly, pours into preheating by step e
In mold, vulcanize 15~25 hours in 90~110 DEG C of baking oven, places 6~9 hours, can be prepared by high temperature resistant polyurethane bullet
Property material.
5. the sealing according to claim 4 processing technology of fire-resistant high-resiliency polyurethane, it is characterized in that: in step a
In, the molecular weight of polytetrahydrofuran is 2000, and the molecular weight of polyester-diol is 2400.
6. the sealing according to claim 4 processing technology of fire-resistant high-resiliency polyurethane, it is characterized in that: in step c,
The hydroxyl value of obtained base polyurethane prepolymer for use as is measured, hydroxyl value need to react again less than 90%, and hydroxyl value is more than or equal to 90% can
Carry out subsequent job.
7. the sealing according to claim 4 processing technology of fire-resistant high-resiliency polyurethane, it is characterized in that: in step d,
Moisture in still air enters in mixed liquor.
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