CN103224606B - Polyurethane node material for submarine oil-gas pipeline interface wet type thermal insulation, and preparation method thereof - Google Patents
Polyurethane node material for submarine oil-gas pipeline interface wet type thermal insulation, and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a polyurethane node material for submarine oil-gas pipeline interface wet type thermal insulation. The polyurethane node material is prepared from a component A and a component B, wherein the component A comprises polyether polyol, a chain extender and a catalyst, the component B is trimerization modified isocyanate or a derivative thereof, a NCO mass content is 10-30% in the component B, and a mass ratio of the component A to the component B is 0.25-6:1. According to the present invention, the used catalyst does not contain mercury, and characteristics of environmental protection, long liquidity, and rapid curing at a late stage are provided; a production cycle is short, a mold temperature is low, and the material is suitable for marine on-site casting operations; and the product contains a trimer structure, and good high temperature resistance stability is provided.
Description
Technical field
The present invention relates to a kind of sea-bottom oil-gas pipeline interface wet type thermal insulation urethane gusset material and preparation method thereof.
Background technology
In ocean energy resources especially oil, gas extraction, the gas hydrate caused for preventing the lower low temperature in sea and the formation of oil wax and blocking pipe, the generation caused the accident, pipe-line must adopt the pipeline with certain thickness heat preservation protective layer to carry, and the protection of this type of pipe main body, insulation and preservative coat complete by specific equipment is prefabricated in factory, the quality comparation of its protective layer and insulation antiseptic layer is reliable.Therefore, in ocean scene process of deployment, the protection of interface is then the key ensureing submerged pipeline safe operation with filling.
The filling of early stage submarine heat insulation pipeline interface, main employing bitumastic+sandstone mixing pouring technology, shape in process and need to be heated to more than 200 DEG C, such meeting easily causes preservative coat to burn or burning, and construction environment smog is large, produce obnoxious flavour, contaminate environment, seawater and marine organisms are also constituted a threat to, and opening-supplementing material intensity low (1.5 ~ 5MPa), affect the integral heat insulation effect of pipeline, be difficult to the safe operation ensureing submerged pipeline, prohibit the use in marine site, local at present.
At present, external widespread use be urethane joint technique, but this joint technique (especially the preparation of joint material) only has the external several companies of minority to grasp.The domestic interfacing about pipeline mainly concentrates on the corrosion-resistant thermal insulation structure design of pipe joint, as 200520103653.9,200520026468.4.About submerged pipeline in-situ interface non-foamed polyure-thane gusset material preparation disclosed in patent less, patent 201210258634.8 discloses a kind of full water open-cell rigid polyurethane foams of submarine pipe joint, urethane foam thermal conductivity is lower, high insulating effect, but rate of closed hole does not reach 100%, cause material water-intake rate high, ultimate compression strength is low, is not suitable for the security application of deep-sea wet type thermal insulation pipe joint.
Summary of the invention
The object of this invention is to provide a kind of sea-bottom oil-gas pipeline interface wet type thermal insulation urethane gusset material and preparation method thereof.
A kind of sea-bottom oil-gas pipeline interface wet type thermal insulation urethane gusset material provided by the present invention, it is made up of component A and B component;
Described component A is made up of polyether glycol, chainextender and catalyzer;
Described B component is trimerization modified isocyanate or derivatives thereof, and in described B component, the mass percentage of NCO is 10 ~ 30%;
The mass ratio of described component A and described B component is 0.25 ~ 6:1.
In above-mentioned urethane gusset material, in described B component, the mass percentage of NCO can be 19.55% ~ 23.09%, 19.55%, 21.72%, 22.55% or 23.09;
The mass ratio of described component A and described B component specifically can be 1.17:1,1.19:1,1.2:1 or 1.28:1.
In above-mentioned urethane gusset material, in described component A, the mass ratio of described polyether glycol, described chainextender and described catalyzer can be 12 ~ 70:2 ~ 20:0.001 ~ 4, specifically can be 459.83 ~ 462.88:68.6 ~ 81.48:2.85,462.88:81.48:2.85,462.43:79.56:2.85,462.73:76.61:2.85 or 459.83:68.6:2.85.
In above-mentioned urethane gusset material, described polyether glycol is made up of polyether glycol I and polyether glycol I I,
The hydroxyl value of described polyether glycol I can be 28 ~ 250mgKOH/g, and as 150 ~ 190mgKOH/g, the hydroxyl value of described polyether glycol I I is 14 ~ 400mgKOH/g, as 50 ~ 60mgKOH/g;
The mass ratio of described polyether glycol I and described polyether glycol I I can be 1 ~ 15:20 ~ 55, specifically can be 47.66:415.22,47.21:415.22,45.51:415.22 or 44.61:415.22.
In above-mentioned urethane gusset material, described polyether glycol I can be plam oil polyvalent alcohol, soybean oil base polyol, castor oil-base polyvalent alcohol, hydroxy-terminated polybutadienes polyvalent alcohol and with 3 functionality little point of alcohol or hydramine or 4 functionality small molecular alcohols be initiator, one or more in the ethylene oxide/propylene oxide polyether glycol that is polymerization single polymerization monomer;
Described polyether glycol I I can be in PTMG, polypropylene glycol, polyoxyethylene glycol and their copolyether one or more.
In above-mentioned urethane gusset material, described chainextender can be 1,4-butyleneglycol, ethylene glycol, propylene glycol, glycol ether, glycerol, TriMethylolPropane(TMP), 1,4-cyclohexanediol, Hydrogenated Bisphenol A, 1,6-hexylene glycol, diethanolamine, trolamine, methyldiethanolamine, diethyl toluene diamine or 3,5-dimethythiotoluene diamine.
In above-mentioned urethane gusset material, described catalyzer is that organic amine catalyzer or its salt are (as triethylene diamine (TEDA), 1,8-diazabicyclo (5,4,0) undecylene-7 or its organic salt (as phenolate, 2-ethylhexoate or formate) or organometallic catalysts (as organotin, organo-bismuth, organic zinc, acetylacetonate nickel or methyl ethyl diketone zirconium), as the catalyzer CT-2X that Aladdin reagent company produces.
In above-mentioned urethane gusset material, described B component specifically can be trimerization modified aliphatic isocyanic ester, trimerization modified aromatic race's isocyanic ester and derivative thereof; Described trimerization modified aliphatic isocyanic ester is made up of aliphatics isocyanide ester and aliphatic poly isocyanide ester tripolymer, the trimerical mass percentage of described aliphatic poly isocyanide ester is 5 ~ 40%, specifically can be 11.79% ~ 37.86%, 11.79%, 15.77%, 21.85% or 37.86%.；
Described trimerization modified aromatic race isocyanide ester is made up of aromatic series isocyanide ester and fragrant adoption isocyanide ester tripolymer, and the trimerical mass percentage of described fragrant adoption isocyanide ester is 5 ~ 40%.
The present invention still further provides the preparation method of above-mentioned urethane gusset material, comprises the steps: described polyether glycol to carry out vacuum-drying; Then in described mixture after drying, add described chainextender and described catalyzer, obtain described component A;
Described B component is added in described component A, is poured into after mixing in the ferrule mold of pipe joint, after solidification, namely obtain described urethane gusset material through the demoulding.
In above-mentioned preparation method, described vacuum drying temperature can be 80 ~ 120 DEG C, and the time can be 1 ~ 4 hour, as vacuum-drying 2.5h at 95 DEG C;
When adding described B component in described component A, the temperature of described component A and described B component all can be 10 ~ 60 DEG C, as 30 DEG C;
In the step of described cast, the temperature of the ferrule mold of described pipe joint can be 40 ~ 150 DEG C, as 80 DEG C.
The present invention has following beneficial effect:
1, used catalyst is without mercury, environmental protection, and flow periods is long, and cured later is fast.
2, with short production cycle, die temperature is low, is applicable to marine cast-in-site operation.
3, goods are containing Trimeric structures, have good heat-resistant stable.
Embodiment
Following embodiment is used for further illustrating Synthesis and applications details of the present invention, does not form the restriction to spirit and scope of the invention.
The experimental technique used in following embodiment if no special instructions, is ordinary method.
Material used in following embodiment, reagent etc., if no special instructions, all can obtain from commercial channels.
Raw material used in following embodiment is as follows:
Polypropylene glycol (PPG), hydroxyl value 50 ~ 60mgKOH/g, Shandong blue star east major company;
PTMG (PTMEG), hydroxyl value 35 ~ 400mgKOH/g, BASF Corp. of Germany;
BDO (BDO), glycol ether (DEG), Shanghai Ling Feng Chemical Co., Ltd.;
Catalyzer CT-2X, Aladdin reagent company;
4,4'-MDI, Hensel steps Shanghai urethane company limited.
NCO-B, be trimerization modification MDI, the technical indicator of modification MDI used in following embodiment is shown in table 1, and wherein, B0 is ester modified MDI, the NCO content of ammonia is 24.69%, not containing tripolymer.
The technical indicator of table 1 modification MDI
Product performance in following embodiment are carried out in accordance with the following methods:
Hardness test: according to testing standard ASTM D2240-04, thickness of sample 6mm(or stackable to 6mm lower than 6mm), widthwise central apart from limit at least 12mm, temperature 23 ± 2 DEG C.During test, sclerometer pressing pin angle keep parallel with table top, pressing press certain speed decline, when pressing stopping after in 1s reading.If sclerometer is equipped with maximum reading telltale, then read lower full-scale reading, get at least 6mm of being separated by and get five points and test respectively, get arithmetical av or intermediate value.
Tensile strength is tested: according to testing standard ASTM D638, sample is dumbbell shape, and thickness is 3.2 ± 0.4mm, and it is 25.00 ± 0.25mm that graticule measures length, temperature 23 ± 2 DEG C, humidity 50 ± 5%.During test, start drawing machine with the scope that speed is 100 ± 50mm/min, record load draws-stretches curve, until sample ruptures in designated area.Each goods at least get five sample tests, get arithmetical av or intermediate value.
Thermogravimetric analysis (TGA): adopt N2 atmosphere, flow is 1mL/min, temperature range 40 DEG C ~ 800, and temperature rise rate is 10 DEG C/min.
Thermo-oxidative ageing is tested: adopt 120 DEG C/60 days, the thermal ageing under aerobic conditions, and the velocity of variation situation of mechanical property (hardness of material, tensile strength, elongation at break) is investigated in contrast.
Number in following embodiment is parts by weight.
Embodiment 1,
In the reactor with vacuum and heating unit, by PPG(415.22 part) and PTMEG (47.66 parts) mix and at 95 DEG C vacuum-drying 2.5h, after Slow cooling cools to 50 DEG C, just dried BDO(81.48 part) and catalyzer CT-2X(2.85 part) add, after mix and blend 15min, vacuum outgas obtains component A.
Control A, B temperature of charge is 30 DEG C, 455.63 parts of NCO-B1 are added in above-mentioned component A, after rapid stirring is evenly degassed, pouring into mould temperature is in the mould of 80 DEG C, obtains submerged pipeline in-situ interface of the present invention with containing isocyanurate ring non-foamed polyure-thane gusset material.
Embodiment 2,
In the reactor with vacuum and heating unit, by PPG(415.22 part), PTMEG (47.21 parts) mix and at 95 DEG C vacuum-drying 2.5h, after Slow cooling cools to 60 DEG C, just dried BDO(79.56 part) and catalyzer CT-2X(2.85 part) add, after mix and blend 15min, vacuum outgas obtains component A.
Control A, B temperature of charge is 30 DEG C, 458 parts of NCO-B2 are added in above-mentioned component A, after rapid stirring is evenly degassed, pouring into mould temperature is in the mould of 80 DEG C, obtains submerged pipeline in-situ interface of the present invention with containing isocyanurate ring non-foamed polyure-thane gusset material.
Embodiment 3,
In the reactor with vacuum and heating unit, by PPG(415.22 part), PTMEG (46.51 parts) mix and at 95 DEG C vacuum-drying 2.5h, after Slow cooling cools to 50 DEG C, just dried BDO(76.61 part) and catalyzer CT-2X(2.85 part) add, after mix and blend 15min, vacuum outgas obtains component A.
Control A, B temperature of charge is 30 DEG C, 461.65 parts of NCO-B3 are added in above-mentioned component A, after rapid stirring is evenly degassed, pouring into mould temperature is in the mould of 80 DEG C, obtains submerged pipeline in-situ interface of the present invention with containing isocyanurate ring non-foamed polyure-thane gusset material.
Embodiment 4,
In the reactor with vacuum and heating unit, by PPG(415.22 part), PTMEG (44.61 parts) mix and at 95 DEG C vacuum-drying 2.5h, after Slow cooling cools to 50 ~ 60 DEG C, just dried BDO(68.6 part) and catalyzer CT-2X(2.85 part) add, after mix and blend 15min, vacuum outgas obtains component A.
Control A, B temperature of charge is 30 DEG C, 471.57 parts of NCO-B4 are added in above-mentioned component A, after rapid stirring is evenly degassed, pouring into mould temperature is in the mould of 80 DEG C, obtains submerged pipeline in-situ interface of the present invention with containing isocyanurate ring non-foamed polyure-thane gusset material.
Comparative example 1,
In the reactor with vacuum and heating unit, by PPG(415.22 part), PTMEG (48.98 parts) mix and at 95 DEG C vacuum-drying 2.5h, after Slow cooling cools to 50 ~ 60 DEG C, just dried BDO(87.02 part) and catalyzer CT-2X(2.85 part) add, after mix and blend 15min, vacuum outgas obtains component A.
Control A, B temperature of charge is 30 DEG C, adds 448.78 parts of ester modified isocyanic ester of B0 ammonia in above-mentioned component A, and after rapid stirring is evenly degassed, pouring into mould temperature is in the mould of 80 DEG C, obtains submerged pipeline in-situ interface non-foamed polyure-thane gusset material of the present invention.
The performance characteristics of the gusset material prepared by comparative example 1 and embodiment 1 to 4 is as shown in table 2.
The performance of table 2 gusset material
Performance variation rate after the heat oxygen aging resistance of table 3 gusset material
Can be learnt by the data in table 2, the tensile strength of gusset material provided by the invention is high, and thermotolerance is better, and can serve the interface construction of ocean heat preservation pipeline, its comprehensive mechanical property performance is better than prior art.
After the heat resistant performance of the gusset material prepared by comparative example 1 and embodiment 1 to 4, velocity of variation is as shown in table 3, can be learnt by the data in table 3, and along with the increase of tripolymer content in gusset material, the heat-proof aging stability of material significantly improves.
Technology described above is protected as the technical scheme that completes, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the Equivalent embodiments of equivalent variations.But every for departing from art solutions content of the present invention, any simple modification, equivalent variations or the remodeling done above said content according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (8)
1. a sea-bottom oil-gas pipeline interface wet type thermal insulation urethane gusset material, is characterized in that: described urethane gusset material is made up of component A and B component;
Described component A is made up of polyether glycol, chainextender and catalyzer; The mass ratio of described polyether glycol, described chainextender and described catalyzer is 12 ~ 70:2 ~ 20:0.001 ~ 4;
Described polyether glycol is made up of polyether glycol I and polyether glycol I I;
The hydroxyl value of described polyether glycol I is 28 ~ 250 mgKOH/g, and the hydroxyl value of described polyether glycol I I is 14 ~ 400 mgKOH/g;
The mass ratio of described polyether glycol I and described polyether glycol I I is 1 ~ 15:20 ~ 55;
Described B component is trimerization modified aromatic race isocyanic ester, and in described B component, the mass percentage of NCO is 10 ~ 30%;
The mass ratio of described component A and described B component is 0.25 ~ 6:1.
2. urethane gusset material according to claim 1, is characterized in that: described polyether glycol I is plam oil polyvalent alcohol, soybean oil base polyol, castor oil-base polyvalent alcohol, hydroxy-terminated polybutadienes polyvalent alcohol and with 3 functionality small molecular alcohols or hydramine or 4 functionality small molecular alcohols be initiator, one or more in the ethylene oxide/propylene oxide polyether glycol that is polymerization single polymerization monomer;
Described polyether glycol I I is one or more in PTMG, polypropylene glycol, polyoxyethylene glycol and their copolyether.
3. urethane gusset material according to claim 1 and 2, it is characterized in that: described chainextender is 1,4-butyleneglycol, ethylene glycol, propylene glycol, glycol ether, glycerol, TriMethylolPropane(TMP), 1,4-cyclohexanediol, Hydrogenated Bisphenol A, 1,6-hexylene glycol, diethanolamine, trolamine, methyldiethanolamine, diethyl toluene diamine or 3,5-dimethythiotoluene diamine.
4. urethane gusset material according to claim 1, is characterized in that: described catalyzer is organic amine catalyzer or its salt or organometallic catalysts.
5. urethane gusset material according to claim 4, is characterized in that: described organic amine catalyzer or its salt are 1,8-diazabicyclo (5,4,0) undecylene-7 or its organic salt.
6. urethane gusset material according to claim 1, it is characterized in that: described trimerization modified aromatic race isocyanic ester is made up of aromatic isocyanate and aromatic poly-isocyanate tripolymer, and the trimerical mass percentage of described aromatic poly-isocyanate is 5 ~ 40%.
7. the preparation method of urethane gusset material described in claim 1, comprises the steps: described polyether glycol to carry out vacuum-drying; Then in described mixture after drying, add described chainextender and described catalyzer, obtain described component A;
Described B component is added in described component A, is poured into after mixing in the ferrule mold of pipe joint, after solidification, namely obtain described urethane gusset material through the demoulding.
8. preparation method according to claim 7, is characterized in that: described vacuum drying temperature is 80 ~ 120 DEG C, and the time is 1 ~ 4 hour;
When adding described B component in described component A, the temperature of described component A and described B component is 10 ~ 60 DEG C;
In the step of described cast, the temperature of the ferrule mold of described pipe joint is 40 ~ 150 DEG C.
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Address after: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Co-patentee after: CNOOC research institute limited liability company Patentee after: China Offshore Oil Group Co., Ltd. Address before: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Co-patentee before: CNOOC Research Institute Patentee before: China National Offshore Oil Corporation |
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