CN105367746A - Preparation method of scratch-resistant MDI and IPDI polymer polyurethane curing agent - Google Patents
Preparation method of scratch-resistant MDI and IPDI polymer polyurethane curing agent Download PDFInfo
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- CN105367746A CN105367746A CN201410414795.0A CN201410414795A CN105367746A CN 105367746 A CN105367746 A CN 105367746A CN 201410414795 A CN201410414795 A CN 201410414795A CN 105367746 A CN105367746 A CN 105367746A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—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
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/672—Dicarboxylic acids and dihydroxy compounds
Abstract
The invention relates to a preparation method of a scratch-resistant MDI and IPDI polymer polyurethane curing agent. The scratch-resistant MDI and IPDI polymer polyurethane curing agent comprises low molecular weight polyester polyol, MDI, IPDI, a catalyst and dimethyl carbonate, and the polyester polyol contains an aromatic ring symmetry structure and has rigidity, so the scraping resistance, the hardness and the wear resistance are improved. The solid content of the MDI and IPDI polymer curing agent prepared in the invention is 50-75%, the NCO content is 8-12%, the viscosity is 1200-2200mPa.s, the free isocyanate content is not greater than 1.0%, and the curing agent contains no aromatic hydrocarbons; and the curing agent has the characteristics of environmental protection, good scratch resistance, good transparency and good yellowing resistance. A polyurethane paint prepared from the curing agent and a hydroxyl component has the characteristics of high glossiness, high hardness and high transparency, a film formed by the paint has the characteristics of good scratch resistance, good levelability, high fullness and good intermiscibility; and the curing agent is specially used in various double-component polyester paints, polyurethane paints, decorative paints and matte paints for woodenware, automobiles, metals and plastics.
Description
Technical field
The present invention relates to a kind of preparation method of polyurethane curing agent, refer more particularly to a kind of scratch resistance MDI and IPDI polymer polyurethane curing agent.
Background technology
At present, conventional on market polymer polyurethane curing agent is containing the noxious solvent such as dimethylbenzene and vinyl acetic monomer in MDI/TMP, MDI/HDI, MDI/TDI product; Solidifying agent contains a certain amount of free monomer HDI and MDI; they are noxious chemicals; chemical property is very active; volatility is high; there is strong impulse smell and lacrimation, after suction, stimulate respiratory system, cause headache bronchitis; serious meeting causes death, and causes severe contamination to environment.
IPDI isophorone diisocyanate is a kind of alicyclic isocyanate, and IPDI reactivity ratio aromatic isocyanate is low, but the speed of response of IPDI and hydroxyl is than fast 4 ~ 5 times of the speed of response of HDI and hydroxyl.Because diphenylmethanediisocyanate MDI photostabilization, yellowing resistance are poor, limit its purposes, and isophorone diisocyanate IPDI has excellent light stability, resistance to xanthochromia and resistance toization moral character altogether, but Costco Wholesale is high.
Summary of the invention
The present invention aims to provide the preparation method of a kind of scratch resistance MDI and IPDI polymer polyurethane curing agent.
In order to solve technical problem recited above, the present invention adopts the economy of diphenylmethanediisocyanate MDI, hypotoxicity and isophorone diisocyanate IPDI excellent performance and low-molecular-weight polyester polyol reaction to make MDI and IPDI polymer polyurethane curing agent; Low-molecular-weight polyester polyvalent alcohol used in the present invention adopts phthalic anhydride, terephthalic acid, m-phthalic acid or derivatives thereof and TMP, dibasic alcohol carries out esterification and forms; Molecular structure in MDI and the IPDI polymer polyurethane curing agent made with this polyester polyol contains symmetrical aromatic ring structure, has rigidity, thus improves scrath resistance, hardness and wear resistance; Add appropriate adipic acid or sebacic acid, improve the snappiness of solidifying agent film forming, reduce solidifying agent viscosity, improve the transparency of solidifying agent.Because IPDI reactivity ratio MDI is low, in order to reduce side reaction, Reaction time shorten simultaneously, adopts polyester polyol to drip mode and carries out.
Polyester polyol molecule amount for polyurethane curing agent controls between Mr800 ~ 2000, and molecular weight is large, reacts easily form polyurethane elastomer with polyisocynate monomer.The product hydroxyl value of polyester polyol controls at 120 ~ 150mgKOH/g, hydroxyl value of polyester polyol is large, the viscosity of solidifying agent is little, favourable to raising NCO content, hydroxyl is low, the polyester polyol polymerization degree (molecular weight) is larger, and the solidifying agent viscosity of synthesis is higher, causes solidifying agent solubility property to be deteriorated; But hydroxyl can not be too high, otherwise solidifying agent cost is also higher.The product acid number of polyester polyol controls at 0.3 ~ 1.0mgKOH/g, and acid number can not be less than below 0.2mgKOH/g, otherwise speed of response is difficult to control too soon, preferably controls at 0.3 ~ 0.6mgKOH/g.
Because dimethylbenzene toxicity is large, reflux solvent during great majority all synthesize without dimethylbenzene work, now all with the vinyl acetic monomer reflux solvent and the letdown solvent dun that compare low toxicity, but vinyl acetic monomer or toxicity is larger, boiling point low (77 DEG C), volatile consumption is large, does large arch dam polyurethane curing agent poorly soluble, viscosity is high, uses inconvenience; The present invention adopts the methylcarbonate of environmental protection to make reflux solvent and letdown solvent dun, and boiling point high (90 DEG C), solvability is good, meets the requirement of large arch dam polyurethane curing agent.
In order to solve technical problem recited above, the present invention takes following technical scheme: the preparation method that the present invention relates to a kind of scratch resistance TDI and IPDI polymer polyurethane curing agent, comprises following component: low-molecular-weight polyester polyvalent alcohol 25 ~ 40%, diphenylmethanediisocyanate 15 ~ 40%, isophorone diisocyanate 12 ~ 25%, DBTL catalyzer 0.05 ~ 0.3%, methylcarbonate 25 ~ 50%; The component of described low-molecular-weight polyester polyvalent alcohol is: phthalic anhydride 10 ~ 25%, or terephthalic acid 10 ~ 25%, adipic acid or sebacic acid 3 ~ 8%, TriMethylolPropane(TMP) 7 ~ 15%, dibasic alcohol 25 ~ 45%, 2,6 di tert butyl 4 methyl phenol 0.5 ~ 1.0%, Sb
2o
3/ DBTL (3/1) catalyzer 0.05 ~ 0.3%, methylcarbonate 5 ~ 12%; Described dibasic alcohol is propylene glycol, glycol ether, the one of neopentyl glycol or its combination.
The present invention proposes the preparation method of a kind of scratch resistance MDI and IPDI polymer polyurethane curing agent, comprises the following steps:
1) low-molecular-weight polyester polyvalent alcohol, is prepared, its preparation technology is as follows: in synthesis reactor, by formula ratio add successively phthalic anhydride, or terephthalic acid, adipic acid or sebacic acid, TriMethylolPropane(TMP), dibasic alcohol, 2,6 di tert butyl 4 methyl phenol, Sb
2o
3/ DBTL (3/1) catalyzer, methylcarbonate, pass into nitrogen 10min, gets rid of the air in still, heat under nitrogen protection and stir; Time when about still temperature rise to 180 DEG C, when starting water outlet, every the acid of 0.5h sampling and measuring, hydroxyl value, continue to be warming up to about 240 DEG C insulations, and to control leaving water temperature(LWT) be 95 ~ 105 DEG C, the reaction times is 1.5 ~ 2h, and aquifer yield reaches more than 90% of theoretical aquifer yield, and during substantially constant, esterification terminates; Then at normal pressure and nitrogen protection borehole cooling to 180 DEG C, stop passing into nitrogen, start to vacuumize, under 0.08MPa vacuum tightness, take out 30min, under 0.09MPa vacuum tightness, take out 30min, then under 0.095MPa vacuum tightness, take out 1h, vacuumize while be warmed up to about 240 DEG C simultaneously, sampling and measuring acid number, hydroxyl value, after reaching requirement, discharging is for subsequent use;
2) scratch resistance MDI and IPDI polymer polyurethane curing agent, is prepared, its preparation technology is as follows: in synthesis reactor, MDI, IPDI and methylcarbonate is added by formula ratio, under agitation be warming up to 50 DEG C, after being uniformly dissolved, drip the low-molecular-weight polyester polyvalent alcohol in step 1, dropwise in 1.5 ~ 2h; So progressively be warming up to 65 ~ 70 DEG C, add DBTL catalyzer, keep reaction 2 ~ 3h, cool to 50 DEG C, take out 1h under vacuo and remove unreacted isocyanate-monomer, be cooled to 40 DEG C, add methylcarbonate latting drown by solid content requirement, sampling and measuring solid content, viscosity, NCO and free isocyanate monomer value, after reaching requirement, discharging is packed.
The scratch resistance MDI that the present invention obtains and IPDI polymer polyurethane curing agent, solid content is 50 ~ 75%, NCO content is 8 ~ 12%, and viscosity is 1200 ~ 2200mPas, free isocyanate≤1.0%, aromatic free; Have that environmental protection, scratch resistance are good, good, the resistance to yellowing feature such as good of the transparency.The polyurethane paint prepared with hydroxy component has high gloss, high rigidity, high transparent, paint film scratch resistance is good, good leveling property, the features such as fullness ratio is high, intermiscibility is good are for special curing agents such as the various bi-component polyester paint such as woodenware, automobile, metal, plastics, polyurethane paint, fancy paint, dumb light paints.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1:
1), the preparation of low-molecular-weight polyester polyvalent alcohol: in synthesis reactor, by formulation weight ratio, add phthalic anhydride 18 parts, m-phthalic acid 13 parts, adipic acid 3.5 parts, TriMethylolPropane(TMP) 11 parts, propylene glycol 15 parts, glycol ether 30 parts, 2,6 di tert butyl 4 methyl phenol 0.5 part, Sb successively
2o
3/ DBTL (3/1) catalyzer 0.1 part, methylcarbonate 8.9 parts, passes into nitrogen 10min, gets rid of the air in still, heats under nitrogen protection and stir; Time when about still temperature rise to 180 DEG C, when starting water outlet, every the acid of 0.5h sampling and measuring, hydroxyl value, continue to be warming up to about 240 DEG C insulations, and to control leaving water temperature(LWT) be 95 ~ 105 DEG C, the reaction times is 1.5 ~ 2h, and aquifer yield reaches more than 90% of theoretical aquifer yield, and during substantially constant, esterification terminates; Then at normal pressure and nitrogen protection borehole cooling to 180 DEG C, stop passing into nitrogen, start to vacuumize, under 0.08MPa vacuum tightness, take out 30min, under 0.09MPa vacuum tightness, take out 30min, then under 0.095MPa vacuum tightness, take out 1h, vacuumize while be warmed up to about 240 DEG C simultaneously, sample that polyester polyol molecule amount is after measured Mr=1000, acid number is 0.5mgKOH/g, hydroxyl value is 132mgKOH/g, meet technical requirements discharging for subsequent use;
2) scratch resistance MDI and IPDI polymer polyurethane curing agent, is prepared, its preparation technology is as follows: in synthesis reactor, diphenylmethanediisocyanate 20 parts, isophorone diisocyanate 20 parts and methylcarbonate 25 parts is added by formula ratio, under agitation be warming up to 50 DEG C, after being uniformly dissolved, drip the low-molecular-weight polyester polyvalent alcohol 35 parts in step 1, dropwise in 1.5 ~ 2h; So progressively be warming up to 65 ~ 70 DEG C, add DBTL catalyzer 0.09 part, keep reaction 2 ~ 3h, cool to 50 DEG C, take out 1h under vacuo and remove unreacted isocyanate-monomer, be cooled to 40 DEG C, add methylcarbonate latting drown by the requirement of solid content 75 ± 1%, sampling and measuring TDI and IPDI polymer polyurethane curing agent solid content are 75.5%, to be 1560mPas, NCO be viscosity 10.6%, free isocyanate≤0.08%, and product meets discharging packaging after technical requirements.
The scratch resistance MDI that this example is obtained and IPDI polymer polyurethane curing agent and MDI/TMP, MDI/HDI, IPDI trimer curing agent application performance contrast.
PU clear lacquer component A formula is as follows: 60% light alkyd resin 60%, 70% Hydroxylated acrylic resin 15%, 60% aldehyde ketone resin 5%, flow agent 0.2%, defoamer 0.2%, PU thinner 19.6%; Component A: 75% solidifying agent B component=1:0.7.
Table 1: the PU clear lacquer detected result of preparation
See from table 1, the performance after MDI and IPDI polymer polyurethane curing agent film forming is better than MDI/TMP, MDI/HDI, IPDI trimer curing agent in hardness, resistance to marring, wear resistance; Suitable with MDI/TMP, MDI/HDI, IPDI trimer curing agent on drying property, the transparency and gloss; Suitable with MDI/HDI at yellowing resistance, be slightly worse than IPDI tripolymer, be better than by force MDI/TMP solidifying agent.
PU dumb light paint component A formula is as follows: 60% Matt alkyd resin 60%, 70% Hydroxylated acrylic resin 10%, flatting silica 5%, dispersion agent 0.5%, anti-settling agent 0.5%, flow agent 0.3%, defoamer 0.2%, PU thinner 24.0%; Component A: 75% solidifying agent B component=1:0.5.
Table 2: the PU dumb light paint detected result of preparation
See from table 1, the performance after MDI and IPDI polymer polyurethane curing agent film forming is better than MDI/TMP, MDI/HDI, IPDI trimer curing agent in hardness, resistance to marring, wear resistance; Suitable with MDI/TMP, MDI/HDI, IPDI trimer curing agent on drying property, the transparency and gloss; Suitable with MDI/HDI at yellowing resistance, be slightly worse than IPDI tripolymer, be better than by force MDI/TMP solidifying agent.
Embodiment 2:
1), the preparation of low-molecular-weight polyester polyvalent alcohol: in synthesis reactor, by formulation weight ratio, add phthalic anhydride 20 parts, terephthalic acid 12 parts, adipic acid 3 parts, TriMethylolPropane(TMP) 10 parts, neopentyl glycol 12 parts, glycol ether 35 parts, 2,6 di tert butyl 4 methyl phenol 0.5 part, Sb successively
2o
3/ DBTL (3/1) catalyzer 0.1 part, methylcarbonate 7.4 parts, passes into nitrogen 10min, gets rid of the air in still, heats under nitrogen protection and stir; Time when about still temperature rise to 180 DEG C, when starting water outlet, every the acid of 0.5h sampling and measuring, hydroxyl value, continue to be warming up to about 240 DEG C insulations, and to control leaving water temperature(LWT) be 95 ~ 105 DEG C, the reaction times is 1.5 ~ 2h, and aquifer yield reaches more than 90% of theoretical aquifer yield, and during substantially constant, esterification terminates; Then at normal pressure and nitrogen protection borehole cooling to 180 DEG C, stop passing into nitrogen, start to vacuumize, under 0.08MPa vacuum tightness, take out 30min, under 0.09MPa vacuum tightness, take out 30min, then under 0.095MPa vacuum tightness, take out 1h, vacuumize while be warmed up to about 240 DEG C simultaneously, sample that polyester polyol molecule amount is after measured Mr=1000, acid number is 0.6mgKOH/g, hydroxyl value is 135mgKOH/g, meet technical requirements discharging for subsequent use;
2) scratch resistance MDI and IPDI polymer polyurethane curing agent, is prepared, its preparation technology is as follows: in synthesis reactor, diphenylmethanediisocyanate 25 parts, isophorone diisocyanate 15 parts and methylcarbonate 25 parts is added by formula ratio, under agitation be warming up to 50 DEG C, after being uniformly dissolved, drip the low-molecular-weight polyester polyvalent alcohol 35 parts in step 1, dropwise in 1.5 ~ 2h; So progressively be warming up to 65 ~ 70 DEG C, add DBTL catalyzer 0.08 part, keep reaction 2 ~ 3h, cool to 50 DEG C, take out 1h under vacuo and remove unreacted isocyanate-monomer, be cooled to 40 DEG C, add methylcarbonate latting drown by the requirement of solid content 65 ± 1%, sampling and measuring TDI and IPDI polymer polyurethane curing agent solid content are 75.2%, to be 1680mPas, NCO be viscosity 10.2%, free isocyanate≤0.08%, and product meets discharging packaging after technical requirements.
The scratch resistance MDI that this example is obtained and IPDI polymer polyurethane curing agent and MDI/TMP, MDI/HDI, IPDI trimer curing agent application performance contrast.
PU clear lacquer component A formula is as follows: 60% light alkyd resin 60%, 70% Hydroxylated acrylic resin 15%, 60% aldehyde ketone resin 5%, flow agent 0.2%, defoamer 0.2%, PU thinner 19.6%; Component A: 75% solidifying agent B component=1:0.7.
Table 3: the PU clear lacquer detected result of preparation
See from table 3, the performance after MDI and IPDI polymer polyurethane curing agent film forming is better than MDI/TMP, MDI/HDI, IPDI trimer curing agent in hardness, resistance to marring, wear resistance; Suitable with MDI/TMP, MDI/HDI, IPDI trimer curing agent on drying property, the transparency and gloss; Suitable with MDI/HDI at yellowing resistance, be slightly worse than IPDI tripolymer, be better than by force MDI/TMP solidifying agent.
PU dumb light paint component A formula is as follows: 60% Matt alkyd resin 60%, 70% Hydroxylated acrylic resin 10%, flatting silica 5%, dispersion agent 0.5%, anti-settling agent 0.5%, flow agent 0.3%, defoamer 0.2%, PU thinner 24.0%; Component A: 75% solidifying agent B component=1:0.5.
Table 4: the PU dumb light paint detected result of preparation
See from table 1, the performance after MDI and IPDI polymer polyurethane curing agent film forming is better than MDI/TMP, MDI/HDI, IPDI trimer curing agent in hardness, resistance to marring, wear resistance; Suitable with MDI/TMP, MDI/HDI, IPDI trimer curing agent on drying property, the transparency and gloss; Suitable with MDI/HDI at yellowing resistance, be slightly worse than IPDI tripolymer, be better than by force MDI/TMP solidifying agent.
Although the present invention has been explained in detail and has quoted embodiment as proof, for those of ordinary skill in the art, the various schemes obviously can made according to above-mentioned explanation, amendment and change, within the scope that all should be included in claim.
Claims (2)
1. scratch resistance MDI and an IPDI polymer polyurethane curing agent, is characterized in that: comprise following component: low-molecular-weight polyester polyvalent alcohol 25 ~ 40%, diphenylmethanediisocyanate 15 ~ 40%, isophorone diisocyanate 12 ~ 25%, DBTL catalyzer 0.05 ~ 0.3%, methylcarbonate 25 ~ 50%; The component of described low-molecular-weight polyester polyvalent alcohol is: phthalic anhydride 10 ~ 25%, or terephthalic acid 10 ~ 25%, adipic acid or sebacic acid 3 ~ 8%, TriMethylolPropane(TMP) 7 ~ 15%, dibasic alcohol 25 ~ 45%, 2,6 di tert butyl 4 methyl phenol 0.5 ~ 1.0%, Sb
2o
3/ DBTL (3/1) catalyzer 0.05 ~ 0.3%, methylcarbonate 5 ~ 12%; Described dibasic alcohol is propylene glycol, glycol ether, the one of neopentyl glycol or its combination.
2. a preparation method for a kind of scratch resistance MDI as claimed in claim 1 and IPDI polymer polyurethane curing agent, is characterized in that: described preparation method, comprising:
1) low-molecular-weight polyester polyvalent alcohol, is prepared, its preparation technology is as follows: in synthesis reactor, by formula ratio add successively phthalic anhydride, or terephthalic acid, adipic acid or sebacic acid, TriMethylolPropane(TMP), dibasic alcohol, 2,6 di tert butyl 4 methyl phenol, Sb
2o
3/ DBTL (3/1) catalyzer, methylcarbonate, pass into nitrogen 10min, gets rid of the air in still, heat under nitrogen protection and stir; Time when about still temperature rise to 180 DEG C, when starting water outlet, every the acid of 0.5h sampling and measuring, hydroxyl value, continue to be warming up to about 240 DEG C insulations, and to control leaving water temperature(LWT) be 95 ~ 105 DEG C, the reaction times is 1.5 ~ 2h, and aquifer yield reaches more than 90% of theoretical aquifer yield, and during substantially constant, esterification terminates; Then at normal pressure and nitrogen protection borehole cooling to 180 DEG C, stop passing into nitrogen, start to vacuumize, under 0.08MPa vacuum tightness, take out 30min, under 0.09MPa vacuum tightness, take out 30min, then under 0.095MPa vacuum tightness, take out 1h, vacuumize while be warmed up to about 240 DEG C simultaneously, sampling and measuring acid number, hydroxyl value, after reaching requirement, discharging is for subsequent use;
2) scratch resistance MDI, is prepared and IPDI polymer polyurethane curing agent technique is as follows: in synthesis reactor, MDI, IPDI and methylcarbonate is added by formula ratio, under agitation be warming up to 50 DEG C, after being uniformly dissolved, drip the low-molecular-weight polyester polyvalent alcohol in step 1, dropwise in 1.5 ~ 2h; So progressively be warming up to 65 ~ 70 DEG C, add DBTL catalyzer, keep reaction 2 ~ 3h, cool to 50 DEG C, take out 1h under vacuo and remove unreacted isocyanate-monomer, be cooled to 40 DEG C, add methylcarbonate latting drown by solid content requirement, sampling and measuring solid content, viscosity, NCO and free isocyanate monomer value, after reaching requirement, discharging is packed.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410414795.0A CN105367746A (en) | 2014-08-21 | 2014-08-21 | Preparation method of scratch-resistant MDI and IPDI polymer polyurethane curing agent |
| PCT/CN2015/080484 WO2016026341A1 (en) | 2014-08-21 | 2015-06-01 | Method for preparing scratch-resistant mdi-ipdi polymer polyurethane curing agent |
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| CN201410414795.0A CN105367746A (en) | 2014-08-21 | 2014-08-21 | Preparation method of scratch-resistant MDI and IPDI polymer polyurethane curing agent |
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| CN115181245B (en) * | 2022-08-16 | 2024-03-15 | 广东鼎立森新材料有限公司 | HDI/IPDI curing agent, preparation method, application and thermosetting PU adhesive film |
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