CN101928376B - Polyurethane elastomer composition and preparation method thereof - Google Patents
Polyurethane elastomer composition and preparation method thereof Download PDFInfo
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- CN101928376B CN101928376B CN 201010265813 CN201010265813A CN101928376B CN 101928376 B CN101928376 B CN 101928376B CN 201010265813 CN201010265813 CN 201010265813 CN 201010265813 A CN201010265813 A CN 201010265813A CN 101928376 B CN101928376 B CN 101928376B
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Abstract
The invention discloses a polyurethane elastomer and a preparation method thereof. The method comprises the following steps: evenly mixing polyurethane prepolymer with curing agent, removing foam, casting and curing to obtain the polyurethane elastomer, wherein the curing agent is composed of at least one of chain extender and cross-linking agent, catalyst and other additives. The Shaw hardness Aof the polyurethane elastomer prepared by the invention is 70-90A, the tensile strength thereof is not less than 14MPa, and the elongation at break thereof is not less than 360%; and the polyurethaneelastomer can resist hydrolysis, meets performance requirements for the spiral strake material in the deep-sea riser vortex-excited oscillation suppression device, and has important application value.
Description
Technical field
The present invention relates to polyurethane elastomeric compositions and preparation method thereof.
Background technology
Standpipe is requisite integral part in the marine oil and gas exploitation, and it is bearing the critical functions such as oil transportation, oil recovery, probing, water filling.When ocean current is flowed through standpipe with certain flow velocity, can alternately form in the standpipe both sides vortex of a pair of fixed symmetrical, the periodicity resistance that this vortex causes can make right cylinder come the flow path direction vibration-generating, i.e. (in-line) vibration or longitudinal vibration in so-called line; Increase along with flow velocity, can alternately form strong vortex in the standpipe both sides, Vortex Shedding can produce the variable force of one-period to standpipe, make standpipe with flow to vertical direction on transverse vibration (cross-flow) occurs, be called again vertical vibration.Meanwhile, the generation of vortex and releasing also can produce the drag force of downbeam to cylinder, be also periodic power; But it does not change direction, just periodic increase and decrease, and this can cause the longitudinal vibration of standpipe.The vibration of structure conversely again stream field exert an influence, vortex is strengthened, the vibration aggravation, the problem of this fluid-structure interaction is known as " vortex-induced vibration ".Vortex-induced vibration is the principal element that causes the marine riser fatigure failure, and it can aggravate the fatigure failure of standpipe, can cause the fracture of standpipe, brings the heavy losses such as oil field stopping production, environmental pollution.
Than the shoaling water, vortex-induced vibration more easily occurs in Deepwater Risers, in order effectively to suppress the generation of Deepwater Risers vortex-induced vibration, usually adopts in the world the method for adding restraining device outside standpipe.The riser vortex induced vibration suppression device mainly contains spiral strake, flow deflector, ribbon, thrust, buoyant mass etc., and the characteristics such as the efficient of shaking is high, installation is convenient, long service life suppress to use in Practical Project more at the Deepwater Risers vortex-induced vibration but the spiral strake is because having.
The material of making the spiral strake has the materials such as rubber, polyethylene, galss fiber reinforced resin, but its wear resistance is relatively poor, can be caused but easily poke during installation the decrease in efficiency of shaking.
Summary of the invention
The purpose of this invention is to provide a kind of polyurethane elastomer and preparation method thereof.
The method for preparing polyurethane elastomer provided by the invention comprises the steps: that with base polyurethane prepolymer for use as and solidifying agent mixing, cast cured explosive after de-bubble obtains described polyurethane elastomer.
In the method, described base polyurethane prepolymer for use as is to be got 40-100 ℃ of reaction 1.0-4.0 hour by polyether glycol and isocyanate compound, the mass ratio of described polyether glycol and described isocyanate compound is 1: 1-6: 1, specifically can be 1.3-5.3: 1,1.3-2.9: 1,1.3-1.6: 1,1.3-1.5: 1,1.5-5.3: 1,1.5-2.9: 1,1.5-1.6: 1,1.6-5.3: 1,1.6-2.9: 1 or 2.9-5.3: 1, preferred 1.5: 1-2.5: 1; This temperature of reaction specifically can be 80 ± 2 ℃, 75 ± 2 ℃, 60 ± 2 ℃, 90 ± 2 ℃, 80-90 ℃, 60-90 ℃, 60-75 ℃, 60-80 ℃, 75-90 ℃ or 75-80 ℃, and the reaction times is specially 2-3.5 hour, 2-2.5 hour, 2-3 hour or 3-3.5 hour; The molecular weight of described base polyurethane prepolymer for use as is 1200-15000, is specially 3000-6000,3300-6000,3500-6000 or 5000-6000, preferred 2000-6000;
Described polyether glycol is Polyoxypropylene diol, polyoxybutylene dibasic alcohol, polyoxygenated tetramethylene dibasic alcohol, polyoxytrimethylene-ethylene oxide dibasic alcohol, polyoxytrimethylene trivalent alcohol, polyoxytrimethylene-ethylene oxide trivalent alcohol; the relative molecular mass of described Polyoxypropylene diol is 1000-4000 (preferred 2000), the relative molecular mass of described polyoxybutylene dibasic alcohol is 1000-4000, the relative molecular mass of described polyoxygenated tetramethylene dibasic alcohol is 1000-3000 (preferred 1000-2000, more preferably 2000), the relative molecular mass of described polyoxytrimethylene-ethylene oxide dibasic alcohol is 1000-4000, the relative molecular mass of described polyoxytrimethylene trivalent alcohol is 3000-8000 (preferred 3000), the relative molecular mass of described polyoxytrimethylene-ethylene oxide trivalent alcohol is 3000-8000.
Described isocyanate compound is diphenylmethanediisocyanate, dicyclohexyl methane diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate (HDI) or the PPDI of tolylene diisocyanate (TDI), diphenylmethanediisocyanate (MDI), polymethylene multi-phenenyl isocyanate, Carbodiimide-Modified; Wherein, the polymethylene multi-phenenyl isocyanate of various public sales all is applicable to the method, as the model that can be available from Yantai Wanhua Polyurethane Co., Ltd is the product of PM-200, the diphenylmethanediisocyanate of various commercially available Carbodiimide-Modifieds all is applicable to the method, as the model that can be available from Yantai Wanhua Polyurethane Co., Ltd is the product of MDI-100LL;
Described solidifying agent comprises at least a in catalyzer, chainextender and linking agent; Described catalyzer is organo-metallic catalyst or organic amine catalyzer, and described organo-metallic catalyst is dibutyl tin laurate, stannous octoate or bismuth carboxylate; Described organic amine catalyzer is triethylenediamine or Tetramethyl Ethylene Diamine; Described chainextender be BDO (Isosorbide-5-Nitrae-BDO), 1,6-hexylene glycol, 3,3 '-two chloro-4,4 '-diphenylmethanediamiand, 3,5-dimethythiotoluene diamine or 2,4-diamino-3,5-dimethyl sulphur-based chlorobenzene; Described linking agent is TriMethylolPropane(TMP) or trolamine.
The mol ratio that contains the group of active hydrogen in described base polyurethane prepolymer for use as in isocyanate groups and described solidifying agent is 0.7-1.2: 1, be specially 0.95-1.2: 1,0.95-1.1: 1,0.95-1.02: 1,0.95-1.0: 1,1.0-1.2: 1,1.0-1.1: 1,1.0-1.02: 1,1.02-1.2: 1,1.02-1.1: 1 or 1.1-1.2: 1, preferred 0.9～1.05: 1; The described group that contains active hydrogen is selected from least a in hydroxyl and amido;
Described solidifying agent is comprised of described catalyzer and described chainextender, the mass ratio of described catalyzer and described chainextender is 0.001-0.5: 3-20, specifically can be 0.01-0.2: 12-19,0.01-0.2: 4.9-19,0.01-0.2: 4.9-12,0.01-0.2: 4.9-27.7,0.01-0.2: 12-27.7,0.01-0.2: 19-27.7,0.05-0.2: 4.9-27.7,0.05-0.2: 12-19,0.05: 27.7,0.01: 4.9,0.01: 12 or 0.2: 19, preferred 0.01-0.2: 10;
Described solidifying agent is comprised of described catalyzer and described linking agent, and the mass ratio of described catalyzer and described linking agent is 0.001-0.5: 5-15, preferred 0.01-0.2: 8;
Described solidifying agent is comprised of described catalyzer, described chainextender and described linking agent, and the mass ratio of described catalyzer, described chainextender and described linking agent is 0.001-0.5: 3-15: 2-5, specifically can be 0.1: 15: 2.4, preferred 0.01-0.2: 6: 3.
Described solidifying agent also comprises at least a in stablizer, antioxidant and pigment, described stablizer is two (2,2,6,6-tetramethyl--4-piperidyl) sebate or 1,6-hexa-methylene two (3,5-di-t-butyl-4-hydroxyl hydrogenated cinnamate), preferred two (2,2,6,6-tetramethyl--4-piperidyl) sebate; Described antioxidant be triglycol two-[3-(3-tertiary butyl-4-hydroxy-5-aminomethyl phenyl) propionic ester], tetramethylene (3,5-di-t-butyl-4-hydroxy phenylpropionic acid) methyl esters or 3,5-di-tert-butyl-hydroxy phenyl propionic acid octadecanol ester, preferred tetramethylene (3,5-di-t-butyl-4-hydroxy phenylpropionic acid) methyl esters; Described pigment is carbon black, titan yellow, phthalein viridescent or organic red, and is preferred organic red.The concrete consumption of stablizer, antioxidant and pigment can add according to actual needs.This solidifying agent can be solidifying agent a or solidifying agent b, described solidifying agent a is comprised of described catalyzer, described chainextender, described linking agent, described stablizer, described antioxidant and described pigment, and described solidifying agent b is comprised of described catalyzer, described chainextender and described linking agent.
In the curing schedule of aforesaid method, temperature is 60～110 ℃, specifically can be 60-100 ℃, 60-90 ℃, 60-80 ℃, 80-100 ℃, 80-90 ℃, 90-100 ℃, 80 ℃, 90 ℃ or 100 ℃, preferred 100 ℃, time is 4～20 hours, specifically can be 12-20 hour, 12-16 hour, 12-14 hour, 14-20 hour, 14-16 hour, 16-20 hours 20 hours, 12 hours, 14 hours or 16 hours, preferred 16 hours.In this curing schedule, what carry out between reactant is vulcanization reaction.
In described de-bubble step, the de-bubble mode is the decompression de-bubble, in described decompression de-bubble step, vacuum tightness is 10-500Pa, specifically can be 20-50Pa, 20-100Pa, 20-300Pa, 50-300Pa, 50-100Pa, 100-300Pa, 20-200Pa, 50-200Pa, 100-200Pa or 200-300Pa, preferred 50-200Pa, the time is 1-5 minute, specifically can be 1-3 minute, 1-2 minute or 2-3 minute, preferred 2-4 minute.
The polyurethane elastomer for preparing according to the method described above and the application in spiral strake material in preparation deep sea vertical pipe vortex-induced vibration suppression device thereof also belong to protection scope of the present invention.
The polyurethane elastomer that the present invention prepares, shore hardness A is 70～90, tensile strength is not less than 14MPa, elongation at break is not less than 360%, hydrolysis satisfies the performance requriements of the spiral strake material in the deep sea vertical pipe vortex-induced vibration suppression device, has important using value.
Embodiment
The invention will be further described below in conjunction with embodiment, but the present invention is not limited to following embodiment.Described in following embodiment, umber is mass fraction.
In embodiment, mechanic property test method used is as follows:
Shore hardness A measures by " the pocket sclerometer penetration hardness of GB/T531-2008 rubber test method ";
Tensile strength and elongation at break are measured by " mensuration of GB/T528-1998 vulcanized rubber or thermoplastic elastomer tensile stress-strain performance ";
Tear strength is measured by " mensuration of GB/T529-1999 vulcanized rubber or thermoplastic elastomer tear strength ";
The Akron abrasion value is measured by " mensuration (falling abrasion machine with Acker) of GB/T1689-1998 vulcanized rubber wear resisting property ".
Embodiment 1
1) getting relative molecular mass is 100 parts of 2000 Polyoxypropylene diols, and 50.6 parts of diphenylmethanediisocyanates (MDI) at 80 ± 2 ℃ of reaction 3.0h, obtain base polyurethane prepolymer for use as, and relative molecular mass is 5000.
2) (0.01 part of 12 parts of Isosorbide-5-Nitraes-BDO) and catalyzer dibutyl tin laurate mix, and obtain solidifying agent to get the chainextender BDO.
3) will be according to step 1) 100 parts of preparation gained base polyurethane prepolymer for use as and step 2) 8.1 parts, preparation gained solidifying agent (in performed polymer-mol ratio that contains the group-OH of active hydrogen in NCO group and solidifying agent is 1.1: 1) mix under 70 ℃, (vacuum tightness is 100Pa in decompression, decompression time is 1 minute) be poured in mould after de-bubble, 60 ℃ were vulcanized 20 hours, and obtained polyurethane elastomer provided by the invention.
According to GB/T528-1998, GB/T531-2008, GB/T529-1999 and GB/T1689-1998, the performance of this polyurethane elastomer is measured, acquired results is as follows: shore hardness A is 82, tensile strength is 15MPa, elongation at break is 370%, tear strength is 71KN/m, and the Akron abrasion value is 0.0768g.
Embodiment 2
1) getting relative molecular mass is 100 parts of 3000 polyoxytrimethylene trivalent alcohols, and 19 parts of tolylene diisocyanates (TDI) at 75 ± 2 ℃ of reaction 3.5h, obtain base polyurethane prepolymer for use as, and relative molecular mass is 6000.
2) get chainextender 3,11 parts of 5-dimethythiotoluene diamines (model is Ethacure 300, available from U.S. Albemarle company) are as solidifying agent.
3) will be according to step 1) 100 parts of preparation gained base polyurethane prepolymer for use as and step 2) 9.2 parts, preparation gained solidifying agent (in performed polymer-contain the group-NH of active hydrogen in NCO group and solidifying agent
2Mol ratio be 1.2: 1) mix under 55 ℃, decompression is poured in mould after (vacuum tightness is 50Pa, and decompression time is 2 minutes) de-bubble, 100 ℃ of sulfurations 12 hours obtain polyurethane elastomer provided by the invention.
According to GB/T528-1998, GB/T531-2008 and GB/T529-1999, the performance of this polyurethane elastomer is measured, acquired results is as follows: shore hardness A is 85, and tensile strength is 17MPa, and elongation at break is 410%, tear strength is 75KN/m, and the Akron abrasion value is 0.0831g.
Embodiment 3
1) getting relative molecular mass is 100 parts of 2000 polyoxygenated tetramethylene dibasic alcohol, and 35 parts of isophorone diisocyanates at 90 ± 2 ℃ of reaction 2.5h, obtain base polyurethane prepolymer for use as, and relative molecular mass is 3500.
2) get chainextender 3,15 parts of 5-dimethythiotoluene diamines (model is Ethacure 300, available from U.S. Albemarle company), chainextender 1,0.2 part of 4 parts of 6-hexylene glycols and catalyzer bismuth carboxylate mix, and obtain solidifying agent.
3) will be according to step 1) 100 parts of preparation gained base polyurethane prepolymer for use as and step 2) 14 parts, preparation gained solidifying agent (in performed polymer-group-OH of containing active hydrogen in NCO group and solidifying agent and-NH
2The mol ratio of mole dosage sum is 1.02: 1) mix at 75 ℃, be poured in mould after decompression (vacuum tightness is 300Pa, and decompression time is 3 minutes) de-bubble, 100 ℃ were vulcanized 14 hours, and obtained polyurethane elastomer provided by the invention.
According to GB/T528-1998, GB/T531-2008 and GB/T529-1999, the performance of this polyurethane elastomer is measured, acquired results is as follows: shore hardness A is 86, and tensile strength is 30MPa, and elongation at break is 450%, tear strength is 85KN/m, and the Akron abrasion value is 0.0325g.
Embodiment 4
1) getting relative molecular mass is that 2000 100 parts of Polyoxypropylene diols, relative molecular mass are 50 parts of 1000 polyoxygenated tetramethylene dibasic alcohol, 93 parts of dicyclohexyl methane diisocyanates (HMDI), at 90 ± 2 ℃ of reaction 2.0h, obtain base polyurethane prepolymer for use as, relative molecular mass is 3000.
2) get chainextender 2,4-diamino-3,0.1 part, the inferior tin of 15 parts of 5-dimethyl sulphur-based chlorobenzenes, 2.4 parts of linking agent TriMethylolPropane(TMP)s, octoate catalyst and pigment are organic, and red (model is CA80705/3111, available from the chemical company limited of Ai Ke (Guangzhou)) 0.8 part mix, obtain solidifying agent.
3) will be according to step 1) 100 parts of preparation gained base polyurethane prepolymer for use as and step 2) 22.1 parts, preparation gained solidifying agent (in performed polymer-group-OH of containing active hydrogen in NCO group and solidifying agent and-NH
2The mol ratio of mole dosage sum is 0.95: 1) mix at 60 ℃, be poured in mould after decompression (vacuum tightness is 20Pa, and decompression time is 1 minute) de-bubble, 90 ℃ were vulcanized 12 hours, and obtained polyurethane elastomer provided by the invention.
According to GB/T528-1998, GB/T531-2008 and GB/T529-1999, the performance of this polyurethane elastomer is measured, acquired results is as follows: shore hardness A is 80, and tensile strength is 20MPa, and elongation at break is 380%, tear strength is 80KN/m, and the Akron abrasion value is 0.0517g.
Embodiment 5
1) getting relative molecular mass is that 2000 100 parts of polyoxygenated tetramethylene dibasic alcohol, relative molecular mass are 100 parts of 1000 polyoxygenated tetramethylene dibasic alcohol, 135 parts of diphenylmethanediisocyanates, at 60 ± 2 ℃ of reaction 0.5h, 80 ± 2 ℃ of reaction 2.0h, obtain base polyurethane prepolymer for use as, relative molecular mass is 3300.
2) get chainextender 1,27.7 parts of 4-butyleneglycols, 0.05 part, the inferior tin of octoate catalyst, stablizer two (2,2,6,6-tetramethyl--4-piperidyl) 2.0 parts of sebates and antioxidant tetramethylene (3,5-di-t-butyl-4-hydroxy phenylpropionic acid) 1.0 parts of methyl esters mix, and obtain solidifying agent.
3) will be according to step 1) 100 parts of preparation gained base polyurethane prepolymer for use as and step 2) 9.2 parts, preparation gained solidifying agent (in performed polymer-mol ratio that contains the group-OH of active hydrogen in NCO group and solidifying agent is 1.0: 1) mix at 80 ℃, (vacuum tightness is 200Pa in decompression, decompression time is 1 minute) be poured in mould after de-bubble, 80 ℃ were vulcanized 16 hours, and obtained polyurethane elastomer provided by the invention.
According to GB/T528-1998, GB/T531-2008 and GB/T529-1999, the performance of this polyurethane elastomer is measured, acquired results is as follows: shore hardness A is 75, and tensile strength is 25MPa, and elongation at break is 400%, tear strength is 83KN/m, and the Akron abrasion value is 0.0310g.
Claims (8)
1. a method for preparing polyurethane elastomer, comprise the steps: that with base polyurethane prepolymer for use as and solidifying agent mixing, cast cured explosive after de-bubble obtains described polyurethane elastomer;
Described base polyurethane prepolymer for use as is to be got 40-100 ℃ of reaction 1.0-4.0 hour by polyether glycol and isocyanate compound, and the mass ratio of described polyether glycol and described isocyanate compound is 1: 1-6: 1; The molecular weight of described base polyurethane prepolymer for use as is 1200-15000;
Described polyether glycol is Polyoxypropylene diol, polyoxybutylene dibasic alcohol, polyoxygenated tetramethylene dibasic alcohol, polyoxytrimethylene-ethylene oxide dibasic alcohol, polyoxytrimethylene trivalent alcohol or polyoxytrimethylene-ethylene oxide trivalent alcohol; The relative molecular mass of described Polyoxypropylene diol is 1000-4000, the relative molecular mass of described polyoxybutylene dibasic alcohol is 1000-4000, the relative molecular mass of described polyoxygenated tetramethylene dibasic alcohol is 1000-3000, the relative molecular mass of described polyoxytrimethylene-ethylene oxide dibasic alcohol is 1000-4000, the relative molecular mass of described polyoxytrimethylene trivalent alcohol is 3000-8000, and the relative molecular mass of described polyoxytrimethylene-ethylene oxide trivalent alcohol is 3000-8000; Described isocyanate compound is diphenylmethanediisocyanate, dicyclohexyl methane diisocyanate, isophorone diisocyanate, hexamethylene diisocyanate or the PPDI of tolylene diisocyanate, diphenylmethanediisocyanate, polymethylene multi-phenenyl isocyanate, Carbodiimide-Modified;
Described solidifying agent comprises at least a in catalyzer, chainextender and linking agent; Described catalyzer is organo-metallic catalyst or organic amine catalyzer, and described organo-metallic catalyst is dibutyl tin laurate, stannous octoate or bismuth carboxylate; Described organic amine catalyzer is triethylenediamine or Tetramethyl Ethylene Diamine; Described chainextender is BDO, 1,6-hexylene glycol, 3,3 '-two chloro-4,4 '-diphenylmethanediamiand, 3,5-dimethythiotoluene diamine or 2,4-diamino-3,5-dimethyl sulphur-based chlorobenzene; Described linking agent is TriMethylolPropane(TMP) or trolamine;
In described curing schedule, temperature is 60～110 ℃, and the time is 4～20 hours.
2. method according to claim 1, it is characterized in that: the mol ratio that contains the group of active hydrogen in described base polyurethane prepolymer for use as in isocyanate groups and described solidifying agent is 0.7-1.2: 1; The described group that contains active hydrogen is selected from least a in hydroxyl and amido;
Described solidifying agent is comprised of described catalyzer and described chainextender, and the mass ratio of described catalyzer and described chainextender is 0.001-0.5: 3-20;
Described solidifying agent is comprised of described catalyzer and described linking agent, and the mass ratio of described catalyzer and described linking agent is 0.001-0.5: 5-15;
Described solidifying agent is comprised of described catalyzer, described chainextender and described linking agent, and the mass ratio of described catalyzer, described chainextender and described linking agent is 0.001-0.5: 3-15: 2-5.
3. method according to claim 1 is characterized in that: described solidifying agent also comprises at least a in stablizer, antioxidant and pigment,
Described stablizer is two (2,2,6,6-tetramethyl--4-piperidyl) sebates or 1,6-hexa-methylene two (3,5-di-t-butyl-4-hydroxyl hydrogenated cinnamate);
Described antioxidant be triglycol two-[3-(3-tertiary butyl-4-hydroxy-5-aminomethyl phenyl) propionic ester], tetramethylene (3,5-di-t-butyl-4-hydroxy phenylpropionic acid) methyl esters or 3,5-di-tert-butyl-hydroxy phenyl propionic acid octadecanol ester;
Described pigment is carbon black, titan yellow, phthalein viridescent or organic red.
4. method according to claim 3, it is characterized in that: described solidifying agent is solidifying agent a or solidifying agent b, described solidifying agent a is comprised of described catalyzer, described chainextender, described linking agent, described stablizer, described antioxidant and described pigment, and described solidifying agent b is comprised of described catalyzer, described chainextender and described linking agent.
5. method according to claim 1, it is characterized in that: in described curing schedule, temperature is 100 ℃, and the time is 16 hours.
6. method according to claim 1 is characterized in that: in described de-bubble step, the de-bubble mode is the decompression de-bubble; In described decompression de-bubble step, vacuum tightness is 10-500Pa, and the time is 1-5 minute.
7. the arbitrary described method of claim 1-6 prepares the gained polyurethane elastomer.
8. the described polyurethane elastomer of claim 7 application in spiral strake material in preparation deep sea vertical pipe vortex-induced vibration suppression device.
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