CN118562091A - Casting polyurethane elastomer and preparation method and application thereof - Google Patents
Casting polyurethane elastomer and preparation method and application thereof Download PDFInfo
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- CN118562091A CN118562091A CN202410599583.8A CN202410599583A CN118562091A CN 118562091 A CN118562091 A CN 118562091A CN 202410599583 A CN202410599583 A CN 202410599583A CN 118562091 A CN118562091 A CN 118562091A
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- polyurethane elastomer
- diphenylmethane diisocyanate
- ether glycol
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- 229920003225 polyurethane elastomer Polymers 0.000 title claims abstract description 30
- 238000005266 casting Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims description 9
- 239000000463 material Substances 0.000 claims abstract description 78
- 229920000909 polytetrahydrofuran Polymers 0.000 claims abstract description 35
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 34
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 34
- IBOFVQJTBBUKMU-UHFFFAOYSA-N 4,4'-methylene-bis-(2-chloroaniline) Chemical compound C1=C(Cl)C(N)=CC=C1CC1=CC=C(N)C(Cl)=C1 IBOFVQJTBBUKMU-UHFFFAOYSA-N 0.000 claims abstract description 28
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims abstract description 27
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229920001610 polycaprolactone Polymers 0.000 claims abstract description 24
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 16
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 16
- 239000004611 light stabiliser Substances 0.000 claims abstract description 16
- 239000004632 polycaprolactone Substances 0.000 claims abstract description 13
- 150000002009 diols Chemical class 0.000 claims abstract description 12
- HIFVAOIJYDXIJG-UHFFFAOYSA-N benzylbenzene;isocyanic acid Chemical class N=C=O.N=C=O.C=1C=CC=CC=1CC1=CC=CC=C1 HIFVAOIJYDXIJG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002250 absorbent Substances 0.000 claims abstract description 5
- 230000002745 absorbent Effects 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000004073 vulcanization Methods 0.000 claims description 20
- 238000004519 manufacturing process Methods 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims description 11
- 238000005070 sampling Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 4
- 239000001023 inorganic pigment Substances 0.000 claims description 3
- 241001112258 Moca Species 0.000 abstract description 20
- 239000013535 sea water Substances 0.000 abstract description 7
- 239000007787 solid Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000005259 measurement Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 64
- 239000003795 chemical substances by application Substances 0.000 description 16
- 238000012360 testing method Methods 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 11
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 9
- 230000001276 controlling effect Effects 0.000 description 8
- 229920001971 elastomer Polymers 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000005060 rubber Substances 0.000 description 4
- AOFIWCXMXPVSAZ-UHFFFAOYSA-N 4-methyl-2,6-bis(methylsulfanyl)benzene-1,3-diamine Chemical compound CSC1=CC(C)=C(N)C(SC)=C1N AOFIWCXMXPVSAZ-UHFFFAOYSA-N 0.000 description 3
- 229920002635 polyurethane Polymers 0.000 description 3
- 239000004814 polyurethane Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- XVSJTVAPLGSCSK-UHFFFAOYSA-N 2,3,6-trimethylbenzenethiol Chemical compound CC1=CC=C(C)C(S)=C1C XVSJTVAPLGSCSK-UHFFFAOYSA-N 0.000 description 2
- 239000004433 Thermoplastic polyurethane Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 2
- BJZYYSAMLOBSDY-QMMMGPOBSA-N (2s)-2-butoxybutan-1-ol Chemical compound CCCCO[C@@H](CC)CO BJZYYSAMLOBSDY-QMMMGPOBSA-N 0.000 description 1
- 239000004970 Chain extender Substances 0.000 description 1
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 230000009878 intermolecular interaction Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001228 polyisocyanate Polymers 0.000 description 1
- 239000005056 polyisocyanate Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
Classifications
-
- 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
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl 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
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
-
- 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
- C08G18/4266—Polycondensates having carboxylic or carbonic ester groups in the main chain prepared from hydroxycarboxylic acids and/or lactones
- C08G18/4269—Lactones
- C08G18/4277—Caprolactone and/or substituted caprolactone
-
- 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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/721—Two or more polyisocyanates not provided for in one single group C08G18/73 - C08G18/80
- C08G18/724—Combination of aromatic polyisocyanates with (cyclo)aliphatic polyisocyanates
-
- 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
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/758—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing two or more cycloaliphatic rings
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
Abstract
The invention discloses a casting polyurethane elastomer, which comprises a material A and a material B, wherein the material A comprises 50-90 parts by weight of polytetrahydrofuran ether glycol, 5-20 parts by weight of polycaprolactone diol, 25-40 parts by weight of liquefied diphenylmethane diisocyanate and 1-10 parts by weight of hydrogenated diphenylmethane diisocyanate; the material B comprises 10 to 25 parts by weight of polytetrahydrofuran ether glycol, 3.5 to 5 parts by weight of 1, 4-butanediol, 7.5 to 20 parts by weight of 4,4' -methylenebis (2-chloroaniline), 0.7 to 1 part by weight of antioxidant, 0.7 to 1 part by weight of ultraviolet absorbent, 0.7 to 1 part by weight of light stabilizer and 1.4 to 1.7 parts by weight of color paste. The invention uses the liquefied MDI to replace the solid MDI, has simple and convenient operation, more accurate measurement and better synthesis of ideal products; meanwhile, MOCA and BDO are adopted to jointly extend and solidify, the proportion of the MOCA and BDO can be adjusted according to actual demands to adjust the operation time for casting small or large products, and the products have the advantages of good rebound resilience, small permanent deformation after being pulled apart, good sea water resistance and the like.
Description
Technical Field
The invention relates to the chemical field, in particular to a casting polyurethane elastomer and a preparation method and application thereof.
Background
The polyurethane elastomer is a high molecular synthetic material with excellent comprehensive performance, and comprises a casting polyurethane elastomer (CPU), a thermoplastic polyurethane elastomer (TPU) and a mixing polyurethane elastomer (MPU), wherein the casting polyurethane elastomer is prepared by reacting a polyalcohol oligomer with polyisocyanate to obtain a prepolymer and then solidifying the prepolymer with a chain-extending cross-linking agent. The wear-resistant steel has the advantages of high strength, high wear resistance, light weight and simple process, and is widely applied to various large fields.
At present, a fender is generally placed at a ship outboard or dock berthing position when a ship lands on the shore, so that impact force of the ship and the dock in the landing or mooring process is relieved, and the ship or the dock is prevented from being damaged. Common fenders are mainly rubber fenders and polyurethane elastomer fenders, and the traditional rubber fenders are mainly used in the field of fenders at present. The rubber fender is formed by pouring natural rubber or synthetic rubber sizing materials in a specific mold after hot melting, and has the defects of high density, large counter force, poor energy absorption effect, pressure resistance, wear resistance, fatigue resistance, ageing resistance and the like, and the rubber fender generally has a service life of about 1-3 years and needs frequent replacement when used for large ships; the polyurethane elastomer fender is a fender which is gradually rising in recent years, and the polyurethane elastomer fender rapidly opens the market due to the advantages of light weight, high strength, good energy absorption, high wear resistance, strong ageing resistance and the like, and plays a very important role in the fender field. However, the operation time is shorter when the polyurethane elastomer is synthesized, the existing polyurethane fenders are small fenders, the problems that products are not fully filled and have defects when large fenders products are cast, and the casting of large fenders products cannot be performed, so that the existing polyurethane fenders are still deficient for large ships and matched wharf fenders. The invention patent CN106378891B provides a production process of polyurethane fender for ships and wharfs, according to which fender products with better performance can be prepared, but the product is cast by using dimethyl thiotoluene only as a chain extender, and as the curing speed of the dimethyl thiotoluene is higher, if the product is cast in a larger scale, the condition that a mould cannot be filled can occur, the product performance can be influenced even the casting failure is directly caused, and if a catalyst for adjusting the reaction speed is added, the degradation of the product is faster, and the service life of the fender is shortened.
Therefore, there is a need to develop a casting polyurethane elastomer with long service life, good control of operation time and better performance, which can be used for casting and manufacturing of the fenders of large ships and matched wharfs.
Noun interpretation:
PTMEG: polytetrahydrofuran ether glycol.
PCL: polycaprolactone diol.
Liquified MDI: liquefying diphenylmethane diisocyanate.
HMDI: hydrogenated diphenylmethane diisocyanate.
BDO:1, 4-butanediol.
MOCA:4,4' -methylenebis (2-chloroaniline).
Disclosure of Invention
In order to solve the technical problems, the invention provides a casting polyurethane elastomer and a preparation method and application thereof.
The aim of the invention is achieved by the following technical scheme:
The casting polyurethane elastomer is characterized by comprising a material A and a material B, wherein the material A comprises 50-90 parts by weight of polytetrahydrofuran ether glycol, 5-20 parts by weight of polycaprolactone diol, 25-40 parts by weight of liquefied diphenylmethane diisocyanate and 5-10 parts by weight of hydrogenated diphenylmethane diisocyanate;
The material B comprises 10 to 25 parts by weight of polytetrahydrofuran ether glycol, 3.5 to 5 parts by weight of 1, 4-butanediol, 7.5 to 20 parts by weight of 4,4' -methylenebis (2-chloroaniline), 0.7 to 1 part by weight of antioxidant, 0.7 to 1 part by weight of ultraviolet absorbent, 0.7 to 1 part by weight of light stabilizer and 1.4 to 1.7 parts by weight of color paste.
Further improved, the antioxidant is 1010, the ultraviolet absorber is UV-328, the light stabilizer is LQ-292, and the color paste is inorganic pigment.
A preparation method of a casting polyurethane elastomer comprises the following steps:
Step one, manufacturing a material A: firstly, placing 50-90 parts by weight of polytetrahydrofuran ether glycol and 5-20 parts by weight of polycaprolactone diol into a reaction vessel at 100-110 ℃ for vacuum defoaming for 2-3 hours, closing heating, adding 1-10 parts by weight of hydrogenated diphenylmethane diisocyanate and 25-45 parts by weight of liquefied diphenylmethane diisocyanate when the temperature is reduced to 50-60 ℃, heating to 65-75 ℃, stirring for reacting for 2-3 hours, sampling and detecting NCO value, and stopping reacting when the NCO value reaches a range from 99% to 101% of a preset value to obtain a material A;
Step two, manufacturing a material B: 10 to 25 parts by weight of polytetrahydrofuran ether glycol, 2 to 5 parts by weight of 1, 4-butanediol, 5 to 18 parts by weight of 4,4 '-methylenebis (2-chloroaniline), 0.1 to 1 part by weight of antioxidant, 0.1 to 1 part by weight of ultraviolet absorbent, 0.1 to 1 part by weight of light stabilizer and 0.5 to 3 parts by weight of color paste are placed in a reaction vessel at 110 to 120 ℃ and after the 4,4' -methylenebis (2-chloroaniline) is completely melted, the temperature is reduced to 100 to 105 ℃ and the vacuum defoaming is carried out for 1 to 2 hours, thus obtaining a material B; step three, pouring and vulcanizing: and (3) uniformly mixing the material A and the material B, then injecting the mixture into a mould preheated to 100-105 ℃ for heat preservation for 1-2 hours to carry out vulcanization to obtain a product, taking the product out of the mould, and then placing the product into an oven at 100-105 ℃ for 24 hours to carry out secondary vulcanization to obtain the casting polyurethane elastomer.
Further improved, the preset value NCO' determining method comprises the following steps:
Wherein: m 1、m2、m3、m4 is the added mass of liquefied diphenylmethane diisocyanate, hydrogenated diphenylmethane diisocyanate, polytetrahydrofuran ether glycol and polycaprolactone diol in the first step; m 1、M2、M3、M4 is the relative molecular mass of the liquefied diphenylmethane diisocyanate, hydrogenated diphenylmethane diisocyanate, polytetrahydrofuran ether glycol, and polycaprolactone diol in step one, respectively.
Further improved, the average molecular weight of the polytetrahydrofuran ether glycol and the polycaprolactone diol are both 2000+/-70.
The use of a method for the preparation of a cast polyurethane elastomer, as described above; the casting polyurethane elastomer is used for manufacturing the fender.
The invention has the beneficial effects that:
1) The invention uses the liquefied MDI to replace the solid MDI, is convenient for metering during use, does not need to be heated and melted in advance, reduces the influence of moisture in the air on the MDI, is simple and convenient to operate, has more accurate metering, and can better synthesize an ideal product.
2) The invention adopts MOCA and BDO to jointly extend and solidify, the operation time can be adjusted by adjusting the proportion of the MOCA and BDO, and the operation time is adjusted according to the actual demand to be used for pouring small or large products.
3) According to the invention, part of the ester bond structure of polycaprolactone is introduced into the soft segment, and compared with the traditional polyether polyol, a plurality of ester bonds with higher bond energy and large cohesive energy are added, so that intermolecular interaction force is larger, and the product has the advantages of good mechanical property, good rebound resilience, small permanent deformation after tearing, good sea water resistance and the like.
Detailed Description
The present invention will be described in further detail with the aim of making the objects, technical solutions and advantages of the invention more apparent.
The present invention will be further illustrated with reference to specific examples, but the present invention is not limited to the following examples. The raw materials used in examples and comparative examples were commercially available raw materials and commercially available raw materials were obtained unless otherwise specified.
PTMEG: PTMG 2000, basf, germany;
PCL: hunan Severe chemical Material Co., ltd., PCL 2202C.
In the embodiment, the antioxidant is 1010, the ultraviolet absorber is UV-328, the light stabilizer is LQ-292, and the color paste is inorganic pigment.
Example 1
And (3) material A manufacturing: adding 50g of PTMEG and 20g of PCL into a four-neck flask, heating the materials to 100 ℃, vacuumizing until the system pressure is less than 0.1KPa, performing vacuum defoaming for 3 hours, closing heating, adding 10g of HMDI and 25g of liquefied MDI when the system is cooled to 55 ℃, controlling the system temperature to 65 ℃ when the temperature is over, stirring and reacting for 3 hours at the temperature, sampling and detecting the NCO value to 7.16%, and stopping the reaction to obtain the prepolymer A material.
And (3) preparing a material B: 20g of PTMEG, 4.8g of BDO, 7.5g of MOCA, 0.7g of antioxidant, 0.7g of ultraviolet absorber, 0.7g of light stabilizer and 1.4g of color paste are placed in a four-neck flask at 110 ℃, after the MOCA is completely melted, the system temperature is reduced to 100 ℃, vacuum is pumped until the system pressure is less than 0.1KPa, and vacuum defoaming is carried out for 2 hours, thus obtaining the curing agent B material.
Pouring and vulcanizing: pouring the curing agent B into the material A to start timing (the timing is stopped when the material turns white and the fluidity is slow and the material flows out in a block shape, the time is the operation time of the formula), pouring the mixture into a mould preheated to 110 ℃ in advance to keep the temperature for 1h for one-stage vulcanization, the operation time is 5 '25', taking the product out of the mould, placing the product in a baking oven at 100 ℃ for 24h for two-stage vulcanization to obtain a final finished product, and placing the product in an environment at 25 ℃ for 7d to test each performance of the product.
Example 2
And (3) material A manufacturing: adding 65g of PTMEG and 15g of PCL into a four-neck flask, heating the materials to 105 ℃, vacuumizing until the system pressure is less than 0.1KPa, performing vacuum defoaming for 3 hours, closing heating, adding 5g of HMDI and 35g of liquefied MDI when the system is cooled to 58 ℃, controlling the system temperature to 68 ℃ when the temperature is up, stirring and reacting for 2.5 hours at the temperature, sampling and detecting the NCO value to 6.96%, and stopping the reaction to obtain the prepolymer A material.
And (3) preparing a material B: 25g of PTMEG, 4g of BDO, 12g of MOCA, 0.8g of antioxidant, 0.8g of ultraviolet absorber, 0.8g of light stabilizer and 1.6g of color paste are placed in a four-neck flask at 110 ℃, after the MOCA is completely melted, the system temperature is reduced to 105 ℃, vacuum is pumped until the system pressure is less than 0.1KPa, and vacuum defoaming is carried out for 2 hours, thus obtaining the curing agent B material.
Pouring and vulcanizing: pouring the curing agent B into the material A for timing, uniformly mixing, pouring into a mould preheated to 105 ℃ in advance for heat preservation for 1.5h for one-stage vulcanization, taking out the product from the mould, placing the product into a 100 ℃ oven for 24h for two-stage vulcanization to obtain a final finished product, and placing the final finished product in a 25 ℃ environment for 7d for testing each performance of the final finished product.
Example 3
And (3) material A manufacturing: adding 80g of PTMEG and 12g of PCL into a four-neck flask, heating the materials to 110 ℃, vacuumizing until the system pressure is less than 0.1KPa, performing vacuum defoaming for 2 hours, closing heating, adding 6g of HMDI and 40g of liquefied MDI when the system is cooled to 60 ℃, controlling the system temperature to 70 ℃ when the temperature is up, stirring and reacting for 2 hours at the temperature, sampling and detecting the NCO value to 6.98%, and stopping the reaction to obtain the prepolymer A material.
And (3) preparing a material B: placing 10g of PTMEG, 5g of BDO, 15g of MOCA, 1g of antioxidant, 1g of ultraviolet absorber, 1g of light stabilizer and 1.7g of color paste into a four-neck flask at 115 ℃, after MOCA is completely melted, vacuumizing until the system pressure is less than 0.1KPa for vacuum defoaming for 2 hours when the system temperature is reduced to 100 ℃, and obtaining the curing agent B material.
Pouring and vulcanizing: pouring the curing agent B into the material A for timing, uniformly mixing, pouring into a mould preheated to 100 ℃ in advance for heat preservation for 2 hours for one-stage vulcanization, taking out the product from the mould, placing the product into a drying oven at 100 ℃ for 24 hours for two-stage vulcanization to obtain a final finished product, and placing the finished product in an environment at 25 ℃ for 7 days for testing each performance of the finished product.
Example 4
And (3) material A manufacturing: adding 90g of PTMEG and 5g of PCL into a four-neck flask, heating the materials to 110 ℃, vacuumizing until the system pressure is less than 0.1KPa, performing vacuum defoaming for 1.5h, closing heating, adding 7g of HMDI and 40g of liquefied MDI when the system is cooled to 53 ℃, controlling the system temperature to 65 ℃ when the temperature is over, stirring and reacting for 2.5h at the temperature, sampling and detecting the NCO value to 6.96%, and stopping reacting to obtain the prepolymer A material.
And (3) preparing a material B: 15g of PTMEG, 3.5g of BDO, 20g of MOCA, 1g of antioxidant, 1g of ultraviolet absorber, 1g of light stabilizer and 1.7g of color paste are placed in a four-neck flask at 120 ℃, after the MOCA is completely melted, the system temperature is reduced to 105 ℃, vacuum is pumped until the system pressure is less than 0.1KPa, and vacuum defoaming is carried out for 1.5 hours, so as to obtain the curing agent B material.
Pouring and vulcanizing: pouring the curing agent B into the material A to start timing (the timing is stopped when the material turns white and the fluidity is slow and the material flows out in a block shape, the time is the operation time of the formula), pouring the mixture into a mould preheated to 105 ℃ in advance to keep the temperature for 1.5h for one-stage vulcanization, the operation time is 3 '37', taking the product out of the mould and placing the product into a drying oven at 100 ℃ for 24h for two-stage vulcanization to obtain a final finished product, and placing the product in an environment at 25 ℃ for 7d to test each performance of the product.
Comparative example 1
And (3) material A manufacturing: adding 60g of PTMEG and 10g of PCL into a four-neck flask, heating the materials to 100 ℃, vacuumizing until the system pressure is less than 0.1KPa, performing vacuum defoaming for 3 hours, closing heating, adding 5g of HMDI and 30g of liquefied MDI when the system is cooled to 55 ℃, controlling the system temperature to 65 ℃ when the temperature is over, stirring and reacting for 3 hours at the temperature, sampling and detecting the NCO value to 7.0%, and stopping the reaction to obtain the prepolymer A material.
And (3) preparing a material B: 15g of PTMEG, 17.1g of dimethyl thiotoluene diamine, 0.7g of antioxidant, 0.7g of ultraviolet absorber, 0.7g of light stabilizer and 1.4g of color paste are placed in a four-neck flask at 100 ℃, and vacuum is pumped until the system pressure is less than 0.1KPa, and vacuum defoaming is carried out for 2 hours, thus obtaining a curing agent B material.
Pouring and vulcanizing: pouring the curing agent B into the material A for timing, uniformly mixing, pouring into a mould preheated to 105 ℃ in advance for heat preservation for 1.5h for one-stage vulcanization, taking out the product from the mould, placing the product in a 100 ℃ oven for 24h for two-stage vulcanization to obtain a final finished product, and placing the final finished product in a 25 ℃ environment for 7d, and testing all properties of the final finished product.
Comparative example 2
And (3) material A manufacturing: adding 60g of PTMEG and 10g of PCL into a four-neck flask, heating the materials to 100 ℃, vacuumizing until the system pressure is less than 0.1KPa, performing vacuum defoaming for 3 hours, closing heating, adding 5g of HMDI and 30g of liquefied MDI when the system is cooled to 55 ℃, controlling the system temperature to 65 ℃ when the temperature is over, stirring and reacting for 3 hours at the temperature, sampling and detecting the NCO value to 7.0%, and stopping the reaction to obtain the prepolymer A material.
And (3) preparing a material B: 15g of PTMEG, 17.1g of dimethyl thiotoluene diamine, 0.7g of antioxidant, 0.7g of ultraviolet absorber, 0.7g of light stabilizer and 1.4g of color paste are placed in a four-neck flask at 100 ℃, the four-neck flask is vacuumized until the system pressure is less than 0.1KPa, the vacuum defoaming is carried out for 2 hours, and then 0.2g of phosphoric acid is added into the four-neck flask to regulate the activity, so as to obtain the curing agent B material.
Pouring and vulcanizing: pouring the curing agent B into the material A for timing, uniformly mixing, pouring into a mould preheated to 105 ℃ in advance for heat preservation for 1.5h for one-stage vulcanization, taking out the product from the mould, placing the product into a 100 ℃ oven for 24h for two-stage vulcanization to obtain a final finished product, and placing the final finished product in a 25 ℃ environment for 7d for testing each performance of the final finished product.
Comparative example 3
And (3) material A manufacturing: adding 65g of PTMEG and 15g of PCL into a four-neck flask, heating the materials to 105 ℃, vacuumizing until the system pressure is less than 0.1KPa, performing vacuum defoaming for 2.5h, closing heating, adding 5g of HMDI and 35g of liquefied MDI when the system is cooled to 57 ℃, controlling the system temperature to 68 ℃ when the temperature is over, stirring and reacting for 3h at the temperature, sampling and detecting the NCO value to 6.98%, and stopping the reaction to obtain the prepolymer A material.
And (3) preparing a material B: 20g of PTMEG, 8.1g of BDO, 0.7g of antioxidant, 0.7g of ultraviolet absorber, 0.7g of light stabilizer and 1.5g of color paste are placed in a four-neck flask at 100 ℃, and vacuum is pumped until the system pressure is less than 0.1KPa, and vacuum defoaming is carried out for 2 hours, thus obtaining a curing agent B material.
Pouring and vulcanizing: pouring the curing agent B into the material A for timing, uniformly mixing, pouring into a mould preheated to 110 ℃ in advance for heat preservation for 1.5h for one-stage vulcanization, taking out the product from the mould, placing the product into a 100 ℃ oven for 24h for two-stage vulcanization to obtain a final finished product, and placing the final finished product in the 25 ℃ environment for 7d, and testing all properties of the final finished product.
Comparative example 4
And (3) material A manufacturing: adding 80g of PTMEG and 12g of PCL into a four-neck flask, heating the materials to 107 ℃, vacuumizing until the system pressure is less than 0.1KPa, performing vacuum defoaming for 2.5 hours, closing heating, adding 6g of HMDI and 40g of liquefied MDI when the system is cooled to 52 ℃, controlling the system temperature to 75 ℃ when the temperature is over, stirring and reacting for 2 hours at the temperature, sampling and detecting the NCO value to 7.01%, and stopping the reaction to obtain the prepolymer A material.
And (3) preparing a material B: 15g of PTMEG, 26.7g of MOCA, 0.9g of antioxidant, 0.9g of ultraviolet absorber, 0.9g of light stabilizer and 1.8g of color paste are placed in a four-neck flask at 120 ℃, after the MOCA is completely melted, the system temperature is reduced to 100 ℃, vacuum is pumped until the system pressure is less than 0.1KPa, and vacuum defoaming is carried out for 1 hour, thus obtaining the curing agent B material.
Pouring and vulcanizing: pouring the curing agent B into the material A for timing, uniformly mixing, pouring into a mould preheated to 105 ℃ in advance for heat preservation for 1.5h for one-stage vulcanization, taking out the product from the mould, placing the product into a 100 ℃ oven for 24h for two-stage vulcanization to obtain a final finished product, and placing the final finished product in a 25 ℃ environment for 7d, and testing all properties of the final finished product.
The method for detecting the performance of the cast polyurethane elastomer test piece comprises the following steps:
judging whether the appearance of the test piece has defects such as large bubbles, unfilling and the like by visual inspection; tensile strength and elongation at break and permanent set of the test pieces were tested according to type 1 test pieces of GB/T528; the hardness of the test piece is tested according to GB/T531.1; the resilience of the test piece was tested according to GB/T1681-2009; the seawater resistance of the test piece was tested according to GB/T1690-2006.
The proportions of the examples and the comparative examples and the results of the performance tests of the examples and the comparative examples are as follows:
In the embodiments 1-4, BDO and MOCA are mixed, chain extended and solidified, the operation time can be controlled by the proportion of BDO and MOCA, and in the operation time, enough operation time can be ensured when a large fender is poured, the problem that the fender is defective due to too fast material solidification during pouring can be effectively avoided, and meanwhile, the final product has excellent mechanical property and better rebound resilience and sea water resistance.
Comparative example 1 uses a chain extension cure with a thioxylylenediamine, which has a very short operating time, only about 1 minute, and results in a final product that is not toppled with defects. After the performance test is carried out on the intact part, the mechanical property, rebound resilience and sea water resistance of the product are better, but the operation time is short, so that the product cannot be applied to pouring of large-scale products.
In comparative example 2, dimethyl thiotoluene diamine is adopted for chain extension and solidification, part of phosphoric acid is added for regulating activity, the operation time is prolonged to 4'42 ", and the product can be used for pouring large-scale products, but all performances of the product are reduced, and particularly, the sea water resistance and permanent deformation due to tearing are seriously reduced.
Comparative example 3 uses pure BDO for chain extension, which has a long operating time and excellent mechanical properties, but has a significant drop in permanent set and rebound.
Comparative example 4 uses MOCA for chain extension curing, and the result is similar to that of pure DMTDA, and the mechanical properties are better, but the operation time is too short to obtain a good product.
In summary, the cast polyurethane elastomer provided by the invention uses liquefied MDI to replace solid MDI, is simple and convenient to operate, has more accurate metering, and can better synthesize an ideal product; meanwhile, MOCA and BDO are adopted to jointly extend and solidify, the proportion of the MOCA and BDO can be adjusted according to actual requirements to adjust the operation time for pouring small or large products; the product of the invention has the advantages of good mechanical property, good rebound resilience, small permanent deformation after being pulled apart, good sea water resistance and the like.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (6)
1. The casting polyurethane elastomer is characterized by comprising a material A and a material B, wherein the material A comprises 50-90 parts by weight of polytetrahydrofuran ether glycol, 5-20 parts by weight of polycaprolactone diol, 25-40 parts by weight of liquefied diphenylmethane diisocyanate and 5-10 parts by weight of hydrogenated diphenylmethane diisocyanate;
The material B comprises 10 to 25 parts by weight of polytetrahydrofuran ether glycol, 3.5 to 5 parts by weight of 1, 4-butanediol, 7.5 to 20 parts by weight of 4,4' -methylenebis (2-chloroaniline), 0.7 to 1 part by weight of antioxidant, 0.7 to 1 part by weight of ultraviolet absorbent, 0.7 to 1 part by weight of light stabilizer and 1.4 to 1.7 parts by weight of color paste.
2. The cast polyurethane elastomer of claim 1, wherein the antioxidant is 1010, the ultraviolet absorber is UV-328, the light stabilizer is LQ-292, and the color paste is an inorganic pigment.
3. The preparation method of the casting polyurethane elastomer is characterized by comprising the following steps:
Step one, manufacturing a material A: firstly, placing 50-90 parts by weight of polytetrahydrofuran ether glycol and 5-20 parts by weight of polycaprolactone diol into a reaction vessel at 100-110 ℃ for vacuum defoaming for 2-3 hours, closing heating, adding 1-10 parts by weight of hydrogenated diphenylmethane diisocyanate and 25-45 parts by weight of liquefied diphenylmethane diisocyanate when the temperature is reduced to 50-60 ℃, heating to 65-75 ℃, stirring for reacting for 2-3 hours, sampling and detecting NCO value, and stopping reacting when the NCO value reaches a range from 99% to 101% of a preset value to obtain a material A;
Step two, manufacturing a material B: 10 to 25 parts by weight of polytetrahydrofuran ether glycol, 2 to 5 parts by weight of 1, 4-butanediol, 5 to 18 parts by weight of 4,4 '-methylenebis (2-chloroaniline), 0.1 to 1 part by weight of antioxidant, 0.1 to 1 part by weight of ultraviolet absorbent, 0.1 to 1 part by weight of light stabilizer and 0.5 to 3 parts by weight of color paste are placed in a reaction vessel at 110 to 120 ℃ and after the 4,4' -methylenebis (2-chloroaniline) is completely melted, the temperature is reduced to 100 to 105 ℃ and the vacuum defoaming is carried out for 1 to 2 hours, thus obtaining a material B;
Step three, pouring and vulcanizing: and (3) uniformly mixing the material A and the material B, then injecting the mixture into a mould preheated to 100-105 ℃ for heat preservation for 1-2 hours to carry out vulcanization to obtain a product, taking the product out of the mould, and then placing the product into an oven at 100-105 ℃ for 24 hours to carry out secondary vulcanization to obtain the casting polyurethane elastomer.
4. A method for preparing a cast polyurethane elastomer as claimed in claim 3, wherein the preset value NCO' is determined as follows:
Wherein: m 1、m2、m3、m4 is the added mass of liquefied diphenylmethane diisocyanate, hydrogenated diphenylmethane diisocyanate, polytetrahydrofuran ether glycol and polycaprolactone diol in the first step; m 1、M2、M3、M4 is the relative molecular mass of the liquefied diphenylmethane diisocyanate, hydrogenated diphenylmethane diisocyanate, polytetrahydrofuran ether glycol, and polycaprolactone diol in step one, respectively.
5. The method for producing a cast polyurethane elastomer according to claim 3, wherein the average molecular weight ranges of the polytetrahydrofuran ether glycol and the polycaprolactone diol are 2000.+ -.70.
6. Use of a method for the preparation of a cast polyurethane elastomer, characterized in that the method for the preparation of a cast polyurethane elastomer is as claimed in any one of claims 3 to 5; the casting polyurethane elastomer is used for manufacturing the fender.
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