CN106883592A - A kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin - Google Patents
A kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin Download PDFInfo
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- CN106883592A CN106883592A CN201710155243.6A CN201710155243A CN106883592A CN 106883592 A CN106883592 A CN 106883592A CN 201710155243 A CN201710155243 A CN 201710155243A CN 106883592 A CN106883592 A CN 106883592A
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- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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Abstract
The invention discloses a kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin, by weight percentage, it is mixed by following raw material components:PPG 1 15%, PEPA 1 15%, isocyanates 5 10%, small molecule polyol 0.5 1%, chain extender 2 4%, end-capping reagent 1 2%, catalyst 0.02 0.5%, antioxidant 0.1 1%, silicone oil 0.5 1%, modified nano powder 2 4%, balance of solvent.The present invention not only has excellent dyeability, and with the good characteristic such as color inhibition, wear-resisting, water-fastness.
Description
Technical field
The present invention relates to a kind of use for synthetic leather resin, the more particularly to a kind of poly- ammonia of super abrasive color inhibition easy dyeing super fiber leather
Ester resin.
Background technology
At present, synthetic leather has largely replaced the natural leather of inadequate resource, is used to make in case and bag, clothes, sofa, automobile
Decorations, footwear leather etc., with vast potential for future development.However, with the raising of people's living standard and aesthetic requirement, consumer is to skin
The requirement of the outward appearance, physical property and feel of leather also more and more higher.
Microfiber synthetic leather, can be with senior natural leather at aspects such as appearance tactile impression, physical characteristic and snugness of fits
Compare favourably.But due to nylon superfine fiber and polyurethane resin in microfiber synthetic leather, structure is different, dyeing difference is big, from
And cause the problem that super fiber leather is difficult to dyeing;And common synthetic leather not color inhibition, not wear-resisting, which also limits synthetic leather
Use.Therefore, microfiber synthetic leather super abrasive color inhibition dyeing resin into the necessary trend for developing.
The content of the invention
It is an object of the invention to provide a kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin, not only have
Excellent dyeability (easy dyeing, fixation are strong, dye uptake is high, colouring is uniform), and with color inhibition, wear-resisting, water-fastness etc.
Good characteristic.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin, by weight percentage, by following raw material group
Divide and be mixed:PPG 1-15%, PEPA 1-15%, isocyanates 5-10%, small molecule polyol 0.5-
1%, chain extender 2-4%, end-capping reagent 1-2%, catalyst 0.02-0.5%, antioxidant 0.1-1%, silicone oil 0.5-1%, are modified
Nano-powder 2-4%, balance of solvent.
The present invention is by nano-powder, organosilicon and the group that can be combined with dyestuff is introduced in polyurethane resin, making
Product improves the anti-wear performance and dyeability of synthetic leather on the basis of common synthesising leather performance is met.The present invention is with poly-
Ethoxylated polyhydric alcohol and PEPA are the main donor of hydroxyl, by nano powder modified, and Isocyanate prepolymers, then through chain extension
Reaction, synthesizes a kind of new polyurethane resin.
The present invention group that can be combined with dyestuff of introducing in PU body structure, makes product to meet synthetic leather basic
While performance requirement, the dyeability of synthetic leather is also improved.α-active hydrogen is introduced in PU body structure special
Treated nano-powder, substantially increases the anti-wear performance of resin.Using aliphatic isocyanates as raw material, and poly-
Antioxidant is added in urethane resin synthesis process, the anti-yellowing property of resin is improve.
Preferably, described PPG be selected from polytetrahydrofuran diol, polyoxypropyleneglycol, tetrahydrofuran-
One or more in propylene oxide copolymer glycols, it is many that described PEPA is selected from polycaprolactone polyol, makrolon
One or more in first alcohol, poly (propylene carbonate) polyalcohol, polyadipate alcohol ester polyol, the PPG and poly-
The number-average molecular weight of ester polyol compound is 1000-4000g/mol.
Preferably, the aliphatic isocyanates are IPDI, the hydrogenation isocyanic acid of phenylmethane two
One or more in ester, hexamethylene diisocyanate.
Preferably, the small molecule polyol is selected from ethylene glycol, propane diols, BDO, 1,6- hexylene glycols
One or more;The chain extender is the combination of diphenylmethanediamiand and N methyldiethanol amine by 1: 0.5-2 mass ratio.
Small molecule polyol is used as polyol chain extender, can improve the molecular weight of resin, increases the hard segment content of resin, is improved
Mechanical property and feel after resin film forming.Chain extender selects the combination of diphenylmethanediamiand and N methyldiethanol amine, is
Because after the combination of both chain extenders, while chain extension, moreover it is possible to improve the dyeability of resin.Diphenylmethanediamiand chain extension
Agent can form urea bond with isocyanates, and urea bond polarity is stronger than urethano, strong with dye molecule adhesion;N methyldiethanol amine
With tertiary amine structure, in acid dye liquor, it can as combine acid dyes anion dye seat, therefore, both chain extensions
The combination of agent, can greatly improve the dyeability of resin.
Preferably, the end-capping reagent is methyl alcohol;The solvent is N ' dinethylformamides.
Preferably, the catalyst is organic bismuth catalyst;The antioxidant is antioxidant 1010;The silicone oil is
End hydroxy polyether modified organic silicon.Antioxidant 1010 has photostability, can guarantee that the transparency and colour stability of product;Institute
Silicone oil is stated for end hydroxy polyether modified polyorganosiloxane compound, by the reaction of terminal hydroxy group and isocyanates, can be in polyurethane material
Organosilicon composition is introduced in material, so as to improve the levelability of resin, pliability, water resistance, slipping, weatherability and feel etc..
Preferably, the modified nano powder is obtained by nano-powder through α-active hydrogen modification, nano-powder choosing
One or more from nano silicon, nano titanium oxide, nano zine oxide, nano aluminium oxide.Nano-powder can
The intensity and modulus of organic polymer composite material are improved to a certain extent.But common nano-powder improve intensity and
While modulus, because weaker with the affinity of organic polymer, the reduction of other performances can be caused.In order to increase nano-powder
With the dispersiveness and compatibility of polyurethane resin, other performances are not reduced while mechanical strength of resin is improved, this project is selected
The nano-powder of α-active hydrogen specially treated, it has good adhesion with polyurethane resin, can be with polyurethane resin
Disperseed well.The nano-powder of α-active hydrogen specially treated is introduced, the wear-resisting of polyurethane resin can be greatly improved
Performance.
Preferably, the α-active hydrogen modification processing method is:Oleic acid and nano-powder are matched somebody with somebody according to 1: 1 mol ratio
It is well dispersed in water than after, is processed 1 hour using the gamma-ray irradiation in 60Coradiation source, radiation dose rate is 9kGy/h, so
Centrifugation afterwards, is washed with deionized, drying.
A kind of preparation method of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin, comprises the following steps:
(1) PEPA, PPG, silicone oil are added into reactor, vacuum dehydration is carried out at 110 DEG C, contain it
Water rate is less than 0.03%;
(2) 60 DEG C are cooled to, to antioxidant, modified nano powder and first time partial solvent is added in reactor, are stirred
It is well mixed;
(3) at 50 DEG C, freely heated up after adding isocyanates, catalyst, then temperature control is in 80 DEG C of prepolymerization reaction 3h;
(4) after the completion of pre-polymerization, 60 DEG C are cooled to, add second partial solvent and small molecule polyol, temperature control is 65
DEG C reaction 2h;
(5) 55 DEG C are cooled to, third time partial solvent and chain extender N methyldiethanol amine is added, temperature control is anti-at 60 DEG C
Answer 1h;
(6) 50 DEG C are cooled to, surplus solvent and chain extender diphenylmethanediamiand is added, temperature control is in 55 DEG C of reactions
1h;
(7) end-capping reagent, reaction temperature control is added to stir 1h at 50-55 DEG C, obtain product.
Preferably, first time partial solvent consumption is the 10% of solvent gross weight, second partial solvent consumption is molten
The 40% of agent gross weight, third time partial solvent consumption is the 30% of solvent gross weight.
The beneficial effects of the invention are as follows:
1st, there is color inhibition, the characteristic such as cold-resistant, wear-resisting, water-fastness after product process hides of the present invention, color inhibition grade up to 4 with
On, abrasion performance value is up to more than 1000 times under 1.5kg pressure, and easy dyeing, dye uptake be high, fixation is strong, and K/S values are up to 8.5
More than.
2nd, the simple production process of product of the present invention, to equipment, environment without strict demand.
3rd, dyeing resin tool has good wearability, and the leather being made of this resin has very strong kishke feel, can be by it
Application field is expanded on footwear leather, luggage leather by common clothing leather.
Specific embodiment
Below by specific embodiment, technical scheme is described in further detail.
In the present invention, if not refering in particular to, raw material and equipment for being used etc. is commercially available or commonly used in the art.
Method in following embodiments, unless otherwise instructed, is the conventional method of this area.
Total embodiment:
A kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin, by weight percentage, by following raw material group
Divide and be mixed:PPG 1-15%, PEPA 1-15%, isocyanates 5-10%, small molecule polyol 0.5-
1%, chain extender 2-4%, end-capping reagent 1-2%, catalyst 0.02-0.5%, antioxidant 0.1-1%, silicone oil 0.5-1%, are modified
Nano-powder 2-4%, balance of solvent.
It is common that described PPG is selected from polytetrahydrofuran diol, polyoxypropyleneglycol, tetrahydrofuran-propylene oxide
One or more in polyglycols, described PEPA is selected from polycaprolactone polyol, polycarbonate polyol, poly- carbonic acid
One or more in sub- propyl ester polyalcohol, polyadipate alcohol ester polyol, the PPG and polyester polyols refine
The number-average molecular weight of compound is 1000-4000g/mol.The aliphatic isocyanates are IPDI, hydrogenation
One or more in methylenebis phenyl isocyanate, hexamethylene diisocyanate.The small molecule polyol is selected from second two
One or more in alcohol, propane diols, BDO, 1,6- hexylene glycols;The chain extender is diphenylmethanediamiand and N-
Methyl diethanolamine presses the combination of 1: 0.5-2 mass ratio.The end-capping reagent is methyl alcohol;The solvent is N ' N- dimethyl formyls
Amine.The catalyst is organic bismuth catalyst (commercially available, the organic bismuth catalyst Dabco MB20 of U.S.'s gas chemical industry);It is described anti-
Oxidant is antioxidant 1010;The silicone oil is that (commercially available, Shanghai Tag polymer technology is limited for end hydroxy polyether modified organic silicon
The organosilicon modifier Tech-2127 of company).
The modified nano powder is obtained by nano-powder through α-active hydrogen modification, and nano-powder is selected from nano-silica
One or more in SiClx, nano titanium oxide, nano zine oxide, nano aluminium oxide.The α-active hydrogen modification side
Method is:It is well dispersed in water after oleic acid and nano-powder are matched according to 1: 1 mol ratio, is penetrated using the γ in 60Coradiation source
Line radiation treatment 1 hour, radiation dose rate is 9kGy/h, is then centrifuged for separating, and is washed with deionized, and is dried.
Preparation method, comprises the following steps:
(1) PEPA, PPG, silicone oil are added into reactor, vacuum dehydration is carried out at 110 DEG C, contain it
Water rate is less than 0.03%;
(2) 60 DEG C are cooled to, to addition antioxidant, modified nano powder and first time partial solvent (solvent in reactor
Gross weight 10%), be uniformly mixed;
(3) at 50 DEG C, freely heated up after adding isocyanates, catalyst, then temperature control is in 80 DEG C of prepolymerization reaction 3h;
(4) after the completion of pre-polymerization, 60 DEG C are cooled to, add second partial solvent (the 40% of solvent gross weight) and small point
Sub- polyalcohol, temperature control reacts 2h at 65 DEG C;
(5) 55 DEG C are cooled to, third time partial solvent (the 30% of solvent gross weight) and chain extender N- methyl two is added
Monoethanolamine, temperature control reacts 1h at 60 DEG C;
(6) 50 DEG C are cooled to, surplus solvent (the 20% of solvent gross weight) and chain extender diphenyl methane two is added
Amine, temperature control reacts 1h at 55 DEG C;
(7) end-capping reagent, reaction temperature control is added to stir 1h at 50-55 DEG C, obtain product.
In specific examples below:Catalyst is organic bismuth catalyst (commercially available, the organic bismuth catalyst of U.S.'s gas chemical industry
Dabco MB20) antioxidant be antioxidant 1010;The silicone oil is end hydroxy polyether modified organic silicon (commercially available, Shanghai
The organosilicon modifier Tech-2127 of Tag Polymer Sciences Ltd.).End-capping reagent is methyl alcohol;The solvent is N ' N- bis-
NMF.
Specific embodiment 1:
A kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin, by the component system of following percentage by weight meter
Into:PPG 4%, PEPA 8%, isocyanates 8.6%, small molecule polyol 0.8%, chain extender 2.2%, envelope
End agent 1.5%, catalyst 0.1%, antioxidant 0.5%, silicone oil 0.5%, modified nano powder 3.5%, remaining is solvent.
In the present embodiment:PPG is polytetrahydrofuran diol, and number-average molecular weight is 2000g/mol;Polyester is more
First alcohol is PEPA HP3020, and number-average molecular weight is 2000g/mol;Isocyanates is the hydrogenation isocyanic acid of phenylmethane two
Ester;Small molecule polyol is Isosorbide-5-Nitrae butanediol;Chain extender is the mixture of diphenylmethanediamiand and N methyldiethanol amine, and
Mass ratio is 1: 1;Modified nano powder be nano silicon and nano titanium oxide mixture (mass ratio is 5: 2) through α-
Active hydrogen modification and obtain.α-active hydrogen modification processing method is:By oleic acid and nano silicon and nano titanium oxide
Mixture matched according to 1: 1 mol ratio after be well dispersed in water, the gamma-ray irradiation treatment using 60Coradiation source is 1 small
When, radiation dose rate is 9kGy/h, is then centrifuged for separating, and is washed with deionized, and is dried.
Preparation method, comprises the following steps successively:
(1) PEPA, PPG, silicone oil are added into reactor, vacuum dehydration is carried out at 110 DEG C, contain it
Water rate is less than 0.03%;
(2) 60 DEG C are cooled to, to added in reactor antioxidant, modified nano powder and partial solvent (solvent total amount
10%), it is uniformly mixed;
(3) at 50 DEG C, freely heated up after adding isocyanates, catalyst, then temperature control is in 80 DEG C of prepolymerization reaction 3h;
(4) after the completion of pre-polymerization, 60 DEG C are cooled to, add partial solvent (the 40% of solvent total amount) and small molecule polyol
Chain extender, temperature control reacts 2h at 65 DEG C;
(5) 55 DEG C are cooled to, partial solvent (the 30% of solvent total amount) and N methyldiethanol amine is added, temperature control is 60
DEG C reaction 1h;
(6) 50 DEG C are cooled to, partial solvent (the 20% of solvent total amount) and diphenylmethanediamiand is added, temperature control is 55
DEG C reaction 1h;
(7) methyl alcohol is added to terminate, reaction temperature control stirs 1h at 50-55 DEG C, obtains product.
Specific embodiment 2:
A kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin, by the component system of following percentage by weight meter
Into:PPG 2%, PEPA 10%, isocyanates 9%, small molecule polyol 0.6%, chain extender 3%, end-blocking
Agent 2%, catalyst 0.05%, antioxidant 0.25%, silicone oil 0.5%, modified nano powder 3%, remaining is solvent.
In the present embodiment:PPG is polyoxypropyleneglycol, and number-average molecular weight is 2000g/mol;Polyester is more
First alcohol is the mixture of polycaprolactone polyol and polycarbonate polyol, and number-average molecular weight is 2000g/mol, its quality
Than 4: 1;Isocyanates is that IPDI is with the mixture for hydrogenating methylenebis phenyl isocyanate, and mass ratio
2∶1;Small molecule polyol is propane diols;Chain extender is the mixture of diphenylmethanediamiand and N methyldiethanol amine, and matter
Amount is than being 2: 1;Modified nano powder is the mixture (mass ratio is 2: 1) of nano silicon and nano aluminium oxide through α-active
Hydrogen modification and obtain.α-active hydrogen modification processing method is:By the mixing of oleic acid and nano silicon and nano aluminium oxide
Thing is well dispersed in water after being matched according to 1: 1 mol ratio, is processed 1 hour using the gamma-ray irradiation in 60Coradiation source, spoke
It is 9kGy/h according to close rate, is then centrifuged for separating, be washed with deionized, dries.
Preparation method, comprises the following steps successively:
(1) PEPA, PPG, silicone oil are added into reactor, vacuum dehydration is carried out at 110 DEG C, contain it
Water rate is less than 0.03%;
(2) 60 DEG C are cooled to, to added in reactor antioxidant, modified nano powder and partial solvent (solvent total amount
10%), it is uniformly mixed;
(3) at 50 DEG C, freely heated up after adding isocyanates, catalyst, then temperature control is in 80 DEG C of prepolymerization reaction 3h;
(4) after the completion of pre-polymerization, 60 DEG C are cooled to, add partial solvent (the 40% of solvent total amount) and small molecule polyol
Chain extender, temperature control reacts 2h at 65 DEG C;
(5) 55 DEG C are cooled to, partial solvent (the 30% of solvent total amount) and N methyldiethanol amine is added, temperature control is 60
DEG C reaction 1h;
(6) 50 DEG C are cooled to, partial solvent (the 20% of solvent total amount) and diphenylmethanediamiand is added, temperature control is 55
DEG C reaction 1h;
(7) methyl alcohol is added to terminate, reaction temperature control stirs 1h at 50-55 DEG C, obtains product.
Specific embodiment 3:
A kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin, by the component system of following percentage by weight meter
Into:PPG 10%, PEPA 3%, isocyanates 6.2%, small molecule polyol 0.7%, chain extender 2.4%,
End-capping reagent 1.8%, catalyst 0.2%, antioxidant 0.6%, silicone oil 0.8%, nano-powder 2.5%, remaining is solvent.
In the present embodiment:PPG is tetrahydrofuran-propylene oxide copolymer glycols, and number-average molecular weight is 1000g/
mol;PEPA is polyadipate BDO ester, and number-average molecular weight is 2000g/mol;Isocyanates is six methylenes
Group diisocyanate;Small molecule polyol is 1,6- hexylene glycols;Chain extender is diphenylmethanediamiand and N methyldiethanol amine
Mixture (mass ratio is 1: 2);Modified nano powder is obtained for nano zine oxide through α-active hydrogen modification.α-active hydrogen
Modification processing method is:It is well dispersed in water after oleic acid and nano zine oxide are matched according to 1: 1 mol ratio, using Co 60
The gamma-ray irradiation of irradiation bomb is processed 1 hour, and radiation dose rate is 9kGy/h, is then centrifuged for separating, and is washed with deionized, and is dried
It is dry..
The preparation method of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin, comprises the following steps successively:
(1) PEPA, PPG, silicone oil are added into reactor, vacuum dehydration is carried out at 110 DEG C, contain it
Water rate is less than 0.03%;
(2) 60 DEG C are cooled to, to added in reactor antioxidant, modified nano powder and partial solvent (solvent total amount
10%), it is uniformly mixed;
(3) at 50 DEG C, freely heated up after adding isocyanates, catalyst, then temperature control is in 80 DEG C of prepolymerization reaction 3h;
(4) after the completion of pre-polymerization, 60 DEG C are cooled to, add partial solvent (the 40% of solvent total amount) and small molecule polyol
Chain extender, temperature control reacts 2h at 65 DEG C;
(5) 55 DEG C are cooled to, partial solvent (the 30% of solvent total amount) and N methyldiethanol amine is added, temperature control is 60
DEG C reaction 1h;
(6) 50 DEG C are cooled to, partial solvent (the 20% of solvent total amount) and diphenylmethanediamiand is added, temperature control is 55
DEG C reaction 1h;
(7) methyl alcohol is added to terminate, reaction temperature control stirs 1h at 50-55 DEG C, obtains product.
Embodiment described above is a kind of preferably scheme of the invention, not makees any formal to the present invention
Limitation, also has other variants and remodeling on the premise of without departing from the technical scheme described in claim.
Claims (10)
1. a kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin, it is characterised in that by weight percentage, by with
Lower raw material components are mixed:PPG 1-15%, PEPA 1-15%, isocyanates 5-10%, small molecule is more
First alcohol 0.5-1%, chain extender 2-4%, end-capping reagent 1-2%, catalyst 0.02-0.5%, antioxidant 0.1-1%, silicone oil 0.5-
1%, modified nano powder 2-4%, balance of solvent.
2. a kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin according to claim 1, it is characterised in that
Described PPG is selected from polytetrahydrofuran diol, polyoxypropyleneglycol, tetrahydrofuran-propylene oxide copolymer glycols
One or more, it is many that described PEPA is selected from polycaprolactone polyol, polycarbonate polyol, poly (propylene carbonate)
One or more in first alcohol, polyadipate alcohol ester polyol, the number of the PPG and polyester polyol compound
Average molecular weight is 1000-4000g/mol.
3. a kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin according to claim 1, it is characterised in that
The aliphatic isocyanates are IPDI, hydrogenation methylenebis phenyl isocyanate, the isocyanide of hexa-methylene two
One or more in acid esters.
4. a kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin according to claim 1, it is characterised in that
The small molecule polyol is selected from one or more in ethylene glycol, propane diols, BDO, 1,6- hexylene glycols;The expansion
Chain agent is the combination of diphenylmethanediamiand and N methyldiethanol amine by 1: 0.5-2 mass ratio.
5. a kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin according to claim 1, it is characterised in that
The end-capping reagent is methyl alcohol;The solvent is N ' dinethylformamides.
6. a kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin according to claim 1, it is characterised in that
The catalyst is organic bismuth catalyst;The antioxidant is antioxidant 1010;The silicone oil is that end hydroxy polyether is modified to be had
Machine silicon.
7. a kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin according to claim 1, it is characterised in that
The modified nano powder is obtained by nano-powder through α-active hydrogen modification, and nano-powder is selected from nano silicon, receives
Rice titanium dioxide, nano zine oxide, one or more in nano aluminium oxide.
8. a kind of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin according to claim 1, it is characterised in that
The α-active hydrogen modification processing method is:Water is well dispersed in after oleic acid and nano-powder are matched according to 1: 1 mol ratio
In, using 60Coradiation source gamma-ray irradiation process 1 hour, radiation dose rate is 9kGy/h, be then centrifuged for separate, spend from
Sub- water washing, drying.
9. a kind of preparation method of super abrasive color inhibition easy dyeing super fiber leather polyurethane resin as claimed in claim 1, its
It is characterised by, comprises the following steps:
(1) PEPA, PPG, silicone oil are added into reactor, vacuum dehydration is carried out at 110 DEG C, make its moisture content
Less than 0.03%;
(2) 60 DEG C are cooled to, to antioxidant, modified nano powder and first time partial solvent is added in reactor, stirring mixes
Uniformly;
(3) at 50 DEG C, freely heated up after adding isocyanates, catalyst, then temperature control is in 80 DEG C of prepolymerization reaction 3h;
(4) after the completion of pre-polymerization, 60 DEG C are cooled to, add second partial solvent and small molecule polyol, temperature control is anti-at 65 DEG C
Answer 2h;
(5) 55 DEG C are cooled to, third time partial solvent and chain extender N methyldiethanol amine is added, temperature control is in 60 DEG C of reactions
1h;
(6) 50 DEG C are cooled to, add surplus solvent and chain extender diphenylmethanediamiand, temperature control to react 1h at 55 DEG C;
(7) end-capping reagent, reaction temperature control is added to stir 1h at 50-55 DEG C, obtain product.
10. preparation method according to claim 9, it is characterised in that first time partial solvent consumption is solvent gross weight
10%, second partial solvent consumption is the 40% of solvent gross weight, and third time partial solvent consumption is solvent gross weight
30%.
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