CN106366291A - Self-emulsifying anionic water-based polyurethane curing agent and preparation method thereof - Google Patents
Self-emulsifying anionic water-based polyurethane curing agent and preparation method thereof Download PDFInfo
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- CN106366291A CN106366291A CN201610966669.5A CN201610966669A CN106366291A CN 106366291 A CN106366291 A CN 106366291A CN 201610966669 A CN201610966669 A CN 201610966669A CN 106366291 A CN106366291 A CN 106366291A
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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
- C08G18/77—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur
- C08G18/78—Nitrogen
- C08G18/7806—Nitrogen containing -N-C=0 groups
- C08G18/7843—Nitrogen containing -N-C=0 groups containing urethane groups
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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
- C08G18/2805—Compounds having only one group containing active hydrogen
- C08G18/288—Compounds containing at least one heteroatom other than oxygen or nitrogen
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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
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3855—Low-molecular-weight compounds having heteroatoms other than oxygen having sulfur
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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
- C08G18/77—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur
- C08G18/78—Nitrogen
- C08G18/79—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates
- C08G18/791—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing isocyanurate groups
- C08G18/792—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing isocyanurate groups formed by oligomerisation of aliphatic and/or cycloaliphatic isocyanates or isothiocyanates
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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
- C08G18/77—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur
- C08G18/78—Nitrogen
- C08G18/79—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates
- C08G18/791—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing isocyanurate groups
- C08G18/794—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing isocyanurate groups formed by oligomerisation of aromatic isocyanates or isothiocyanates
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/08—Polyurethanes from polyethers
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a self-emulsifying anionic water-based polyurethane curing agent and a preparation method thereof. The self-emulsifying anionic water-based polyurethane curing agent comprises the following raw materials in percentage by weight: 75-85% of isocyanate monomer and/or derivatives thereof, 2-3% of sulfonic acid derivatives, 10-15% of ether ester solvent and 2-3% of other aids. Various indexes of the self-emulsifying anionic water-based polyurethane curing agent satisfy the Chinese standard, and thus, the curing agent belongs to environment-friendly polyurethane. The self-emulsifying anionic water-based polyurethane curing agent can be produced by a general prepolymer production facility without adding any new facility, has the characteristics of low facility cost and simple operation process, and does not need abundant energies in the treatment process.
Description
Technical field
The invention belongs to the polyurethane coating technical field of environment-friendly type, more particularly, to a kind of sulfonate type self-emulsifying type cloudy from
Sub- water-based polyurethane curing agent and preparation method thereof.
Background technology
With the increase of mankind's environmental consciousness, it is inevitable becoming that water-base polyurethane material replaces traditional solvent borne polyurethane
Gesture and needs.Water-based polyurethane curing agent, with water as disperse medium, has few solvent or solvent-free, odorless, pollution-free, no
The features such as combustion and other emulsions easily blend, are conducive to modification, has been widely used in adhesive, coating, paper coating, leather
In the products such as finishing agent.
In recent years, the Fire Prevention Act that the environment pressure from public opinion due to preserving our planet grows with each passing day and some developed countries work out
Rule and the appearance of solvent regulation, limit the use of solvent borne polyurethane, promote polyurethane material research worker all over the world to amass
Pole carries out exploitation and the research of water-based polyurethane curing agent, and then the firming agent of aqueous polyurethane also produces therewith and quickly sends out
Exhibition.
Water-based polyurethane curing agent is to introduce hydrophilic group on the basis of conventional urethane firming agent to improve poly- isocyanide
Acid esters, to make it easier to emulsion dispersion in water, and keeps certain stability.Its advantage is without solvent, environment-protecting asepsis, glues
Degree low, be easily scattered in waterborne polymeric.Conventional method of modifying is direct emulsion process and hydrophilic modifying.Directly emulsion process is
Hydrophilic segment in finger polyurethane molecular or group content seldom, are not enough to self emulsifying, or thoroughly do not contain parent in its chain
Water composition, therefore need additional emulsifying agent, rely on external force could obtain emulsion.Hydrophilic modifying method refers in base polyurethane prepolymer for use as
It is introduced directly into hydrophilic group in strand, or is introduced into the chain extender containing hydrophilic group, then neutralized into salt, gained
Hydrophilic modifying polyurethane can directly be dispersed in water and form stable polyaminoester emulsion.Directly emulsion process has size not
Deng the shortcomings of the compatibility is poor.Therefore the present invention adopts hydrophilic modifying method to synthesize the firming agent of aqueous polyurethane.At present, most of
Produce water-based polyurethane curing agent be all obtain relatively low admittedly contain, the product of relatively low nco active group, such as patent documentation
Cn200910042107, cn201410657845, cn201210065431 etc..
Content of the invention
In order to overcome the deficiencies in the prior art, one of the object of the invention is to provide a kind of self-emulsifying type anion aqueous poly-
Urethane firming agent.
The second object of the present invention is to provide a kind of preparation method of self-emulsifying type anion aqueous polyurethane firming agent,
Have the characteristics that equipment cost is low, simple to operate, and in processing procedure, be required for substantial amounts of reagent and the energy.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of self-emulsifying type anion aqueous polyurethane firming agent, including following raw material by weight:
Isocyanates monomer and/or its derivant 70-90%；
Sulfonic derivative 1-5%；
Solvent of ether ester type 0-20%；
Other auxiliary agents 1-5%.
Preferably, described self-emulsifying type anion aqueous polyurethane firming agent includes following raw material by weight:
Isocyanates monomer and/or its derivant 80-85%；
Sulfonic derivative 2-3%；
Solvent of ether ester type 10-15%；
Other auxiliary agents 2-3%.
Preferably, described isocyanide acrylic monomer includes toluene di-isocyanate(TDI), di-isocyanate, and diphenyl methane two is different
Cyanate, isophorone diisocyanate, bicyclo- one or more of dicyclohexylmethane diisocyanate.
Preferably, described isocyanates analog derivative includes the addition product of diisocyanates, the trimerization of two isocyanide acids
Body, one or more of biuret of the polymer of diisocyanates or fatty diisocyanate.
Preferably, described sulfonic derivative includes a monohydroxylic sulfonic acid, monohydroxylic sulfonate, dihydroxylic sulphur
Acid, dihydroxylic sulfonate, multi-hydroxy sulfonic acid, one or more of multi-hydroxy sulfonate.
Preferably, described isocyanates monomer and/or its derivant include weight than the isocyanates list for 0-20%
Body and the isocyanate derivates of 80-100%.
Preferably, described sulfonic derivative includes weight than the monohydroxylic sulfonic acid for 80%-100% and 0%-20%
Dihydroxylic sulfonic acid.
Preferably, described solvent of ether ester type is propylene glycol methyl ether acetate, dipropylene glycol methyl ether acetate, propylene-glycol ethyl ether
One or more of acetate, propandiol butyl ether acetate.
Preferably, other auxiliary agents described are n- methyl pyrrolidone, n, n dimethylformamide, dibutyl tin laurate,
Stannous octoate, n, n dimethyl cyclohexyl amine, triethylenediamine, triethylamine, n, n- tetramethyl propane diamine, tripropylamine, diethanol
Amine, triethanolamine, one or more of β-(3,5- di-tert-butyl-hydroxy phenyl) propionate.
The preparation method of above-mentioned self-emulsifying type anion aqueous polyurethane firming agent, comprises the following steps:
(1) weigh raw material by weight；
(2) isocyanates monomer and/or its derivant, ether alcohols solvent, other auxiliary agents are put in reactor, to anti-
Kettle is answered to be heated, heating and temperature control, at 55-60 DEG C, is stirred to the material in reactor during heating, stirs
Mix speed at 50 revs/min, make the material in reactor fully react 1-4h；
(3) add sulfonic derivative, temperature is risen to 70-80 DEG C, in heating process, the material in reactor is entered
Row stirring, makes the material in reactor fully react 2-6h, obtains uniform solution；
(4) stop heating, cool to 55-60 DEG C, be incubated 1-1.5h, filtering and discharging.
The invention has the beneficial effects as follows: the present invention is primarily introduced into hydrophilic group to improve polyisocyanate, so that it is easy
Emulsion dispersion in Yu Shui, and keep certain stability.Its advantage is few with or without solvent, environment-protecting asepsis, viscosity is low, pole
It is easily dispersed in waterborne polymeric.The present invention adopts hydrophilic modifying method to synthesize the firming agent of aqueous polyurethane.The present invention need not enter
Any post processing of row；Apply general prepolymer production equipment can produce, new equipment need not be increased, have equipment cost low,
Feature simple to operate, and in processing procedure, it is required for the substantial amounts of energy.
Specific embodiment
For being best understood from the present invention, with reference to embodiment, the present invention will be described in detail, but application claims
The scope of protection is not limited to the scope that embodiment represents.
Embodiment 1
A kind of self-emulsifying type anion aqueous polyurethane firming agent, is prepared from by following methods:
Add 384g in a 500ml four-hole boiling flask equipped with the protection of agitating device, thermometer and logical nitrogen successively
Diisocyanate, 3gn, n- tetramethyl propane diamine, 3g triethylamine, 100g propylene-glycol ethyl ether acetate, 0.2g β-(tertiary fourth of 3,5- bis-
Base -4- hydroxy phenyl) propionate.Start stirring simultaneously and heat, temperature control is incubated 2h at 60 DEG C；Add 10g
Hydroxyethylsulfonic acid., then temperature is risen to 80 DEG C and is incubated 2h；Then cool the filtering and discharging to 60 DEG C of insulation 1h, obtains and produces
Product.Related using gb 24410-2009 " limits of harmful substances in indoor decorating and refurnishing materials water-borne wood coating " standard detection
Project, testing result see table 1.
The testing result of table 1 embodiment 1:
Embodiment 2
A kind of self-emulsifying type anion aqueous polyurethane firming agent, is prepared from by following methods:
Add 384g different successively in a 500ml four-hole boiling flask equipped with the protection of agitating device, thermometer and logical nitrogen
Isophorone diisocyanate, 1g dibutyl tin laurate, 5gn, n dimethyl cyclohexyl amine, 100g propandiol butyl ether acetate,
0.2g β-(3,5- di-tert-butyl-hydroxy phenyl) propionate.Start stirring simultaneously and heat, temperature control is 60
DEG C insulation 2h；Add 15g aminoethane sulfonic acid sodium, then temperature is risen to 80 DEG C and is incubated 2h；Then cool and be incubated to 60 DEG C
Filtering and discharging after 1h, obtains product.Using gb 24410-2009 " nuisance in indoor decorating and refurnishing materials water-borne wood coating
Matter is limited the quantity ", testing result see table 2.
The testing result of table 2 embodiment 2:
Embodiment 3
A kind of self-emulsifying type anion aqueous polyurethane firming agent, is prepared from by following methods:
Add 384g in a 500ml four-hole boiling flask equipped with the protection of agitating device, thermometer and logical nitrogen successively
Diisocyanate trimer, 3g dibutyl tin laurate, 100g propylene glycol methyl ether acetate, 0.2g β-(3,5- di-t-butyl-
4- hydroxy phenyl) propionate.Start stirring simultaneously and heat, temperature control is incubated 2h at 60 DEG C；Add 12g hydroxyl second
Base sodium sulfonate, then temperature is risen to 80 DEG C and is incubated 2h；Then cool the filtering and discharging to 60 DEG C of insulation 1h, obtains and produces
Product.Related using gb 24410-2009 " limits of harmful substances in indoor decorating and refurnishing materials water-borne wood coating " standard detection
Project, testing result see table 3.
The testing result of table 3 embodiment 3:
Embodiment 4
A kind of self-emulsifying type anion aqueous polyurethane firming agent, is prepared from by following methods:
Add 76.8g in a 500ml four-hole boiling flask equipped with the protection of agitating device, thermometer and logical nitrogen successively
Diisocyanate, 307.2g toluene diisocyanate trimer, 3gn, n- tetramethyl propane diamine, 3g triethylamine, 100g propylene glycol second
Ether acetate, 0.2g β-(3,5- di-tert-butyl-hydroxy phenyl) propionate.Start stirring simultaneously and heat, temperature
Degree controls in 60 DEG C of insulation 2h；Add 8g hydroxyethylsulfonic acid., 2g dihydroxylic sulfonic acid, then temperature is risen to 80 DEG C of insulation 2h；So
After cool to 60 DEG C insulation 1h after filtering and discharging, obtain product.Using gb 24410-2009 " indoor decorating and refurnishing materials
Limits of harmful substances in water-borne wood coating " standard detection relevant item, testing result see table 1:
The testing result of table 1 embodiment 1
Embodiment 5
A kind of self-emulsifying type anion aqueous polyurethane firming agent, is prepared from by following methods:
Add 76.8g in a 500ml four-hole boiling flask equipped with the protection of agitating device, thermometer and logical nitrogen successively
Diisocyanate, 307.2g toluene diisocyanate trimer, 3gn, n- tetramethyl propane diamine, 3g triethylamine, 100g propylene glycol second
Ether acetate, 0.2g β-(3,5- di-tert-butyl-hydroxy phenyl) propionate.Start stirring simultaneously and heat, temperature
Degree controls in 60 DEG C of insulation 2h；Add 10g hydroxyethylsulfonic acid., then temperature is risen to 80 DEG C of insulation 2h；Then cool to 60
DEG C insulation 1h after filtering and discharging, obtain product.Using gb 24410-2009 " in indoor decorating and refurnishing materials water-borne wood coating
Limits of harmful substances " standard detection relevant item, testing result is by table 5:
The testing result of table 5 embodiment 5
Embodiment 6
A kind of self-emulsifying type anion aqueous polyurethane firming agent, is prepared from by following methods:
Add 76.8g in a 500ml four-hole boiling flask equipped with the protection of agitating device, thermometer and logical nitrogen successively
Diisocyanate, 307.2g toluene diisocyanate trimer, 3gn, n- tetramethyl propane diamine, 3g triethylamine, 100g propylene glycol second
Ether acetate, 0.2g β-(3,5- di-tert-butyl-hydroxy phenyl) propionate.Start stirring simultaneously and heat, temperature
Degree controls in 60 DEG C of insulation 2h；Add 8g hydroxyethylsulfonic acid., 2g trihydroxylic sulfonic acid, then temperature is risen to 80 DEG C and is incubated 2h；
Then cool the filtering and discharging to 60 DEG C of insulation 1h, obtains product.Using gb 24410-2009 " indoor decorating material
Limits of harmful substances in material water-borne wood coating " standard detection relevant item, testing result is by table 6:
The testing result of table 6 embodiment 6
The physical parameter of example 1-6 and filming performance:
By physical performance data and the filming performance of embodiment, from alkali resistance and resistance to alcohol explanation monohydroxylic sulfonic acid and binary
Hydroxyl sulfoacid compounds, or monohydroxylic sulfonic acid compounds the film forming degree of cross linking after the firming agent preparing with trihydroxylic sulfonic acid
Improve and improve thus result in physical property, and the degree of cross linking of the firming agent being prepared using single monohydroxylic sulfonic acid is
Decline thus to result in physical property relatively low.
The self-emulsifying type anion aqueous polyurethane the firming agent above embodiment of the present invention being provided and preparation method, enter
Go and be discussed in detail, specific case used herein has been set forth to the principle of the present invention and embodiment, above enforcement
The explanation of example is only intended to help and understands the method for the present invention and its core concept；General technology people simultaneously for this area
Member, according to the thought of the present invention, all will change in specific embodiments and applications, in sum, this explanation
Book content should not be construed as limitation of the present invention.
Claims (10)
1. a kind of self-emulsifying type anion aqueous polyurethane firming agent is it is characterised in that include following raw material by weight:
Isocyanates monomer and/or its derivant 70-90%；
Sulfonic derivative 1-5%；
Solvent of ether ester type 0-20%；
Other auxiliary agents 1-5%.
2. self-emulsifying type anion aqueous polyurethane firming agent according to claim 1 is it is characterised in that include following pressing
The raw material of weight ratio meter:
Isocyanates monomer and or derivatives thereof 80-85%；
Sulfonic derivative 2-3%；
Solvent of ether ester type 10-15%；
Other auxiliary agents 2-3%.
3. self-emulsifying type anion aqueous polyurethane firming agent according to claim 1 and 2 is it is characterised in that described different
Cyanogen acrylic monomer includes toluene di-isocyanate(TDI), di-isocyanate, methyl diphenylene diisocyanate, isophorone two isocyanide
Acid esters, bicyclo- one or more of dicyclohexylmethane diisocyanate.
4. self-emulsifying type anion aqueous polyurethane firming agent according to claim 1 and 2 is it is characterised in that described different
Cyanate derivant includes the addition product of diisocyanates, the trimer of two isocyanide acids, the poly of diisocyanates
One or more in the biuret of body or fatty diisocyanate.
5. self-emulsifying type anion aqueous polyurethane firming agent according to claim 1 and 2 is it is characterised in that described sulphur
Acid derivative includes a monohydroxylic sulfonic acid, monohydroxylic sulfonate, dihydroxylic sulfonic acid, and dihydroxylic sulfonate is polynary
Hydroxyl sulfoacid, one or more of multi-hydroxy sulfonate.
6. self-emulsifying type anion aqueous polyurethane firming agent according to claim 1 and 2 is it is characterised in that described different
Cyanate monomer and/or its derivant include the Carbimide. that weight is than the isocyanates monomer for 0-20% and 80-100%
Esters derivative.
7. self-emulsifying type anion aqueous polyurethane firming agent according to claim 5 is it is characterised in that described sulphonic acids
Derivant includes the dihydroxylic sulfonic acid that weight is than the monohydroxylic sulfonic acid for 80%-100% and 0%-20%.
8. self-emulsifying type anion aqueous polyurethane firming agent according to claim 1 and 2 is it is characterised in that described ether
Esters solvent is propylene glycol methyl ether acetate, dipropylene glycol methyl ether acetate, propylene-glycol ethyl ether acetate, propandiol butyl ether acetic acid
One or more of ester.
9. self-emulsifying type anion aqueous polyurethane firming agent according to claim 1 and 2 it is characterised in that described its
His auxiliary agent is n- methyl pyrrolidone, n, n dimethylformamide, dibutyl tin laurate, stannous octoate, n, n diformazan basic ring
Amine, triethylenediamine, triethylamine, n, n- tetramethyl propane diamine, tripropylamine, diethanolamine, triethanolamine, β-(3,5- bis-
One or more of tert-butyl-hydroxy phenyl) propionate.
10. the preparation method of the self-emulsifying type anion aqueous polyurethane firming agent according to any one of claim 1-9,
It is characterized in that, comprise the following steps:
(1) weigh raw material by weight；
(2) isocyanates monomer and/or its derivant, ether alcohols solvent, other auxiliary agents are put in reactor, to reactor
Heated, heating and temperature control, at 55-60 DEG C, is stirred to the material in reactor during heating, stirring speed
Degree, at 50 revs/min, makes the material in reactor fully react 1-4h；
(3) add sulfonic derivative, temperature is risen to 70-80 DEG C, in heating process, the material in reactor is stirred
Mix, make the material in reactor fully react 2-6h, obtain uniform solution；
(4) stop heating, cool to 55-60 DEG C, be incubated 1-1.5h, filtering and discharging.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107082860A (en) * | 2017-04-25 | 2017-08-22 | 周建明 | Self-emulsifying waterborne polyurethane curing agent and preparation method thereof |
| CN107778447A (en) * | 2017-11-13 | 2018-03-09 | 广东聚盈化工有限公司 | A kind of aqueous one-component moisture polyurethane curing agent and preparation method thereof |
| WO2019080700A1 (en) * | 2017-10-24 | 2019-05-02 | 佛山市精信汇明科技有限公司 | Environment-friendly polyurethane curing agent, preparation method therefor and uses thereof |
| CN109897160A (en) * | 2019-01-10 | 2019-06-18 | 襄阳精信汇明科技股份有限公司 | Blocked polyurethane curing agent emulsion and preparation method and application thereof |
| JP2019189866A (en) * | 2018-04-25 | 2019-10-31 | コベストロ、ドイチュラント、アクチエンゲゼルシャフトＣｏｖｅｓｔｒｏ Ｄｅｕｔｓｃｈｌａｎｄ Ａｇ | Ionically hydrophilized polyisocyanates and radical scavengers and/or peroxide decomposers |
| CN110396165A (en) * | 2018-04-25 | 2019-11-01 | 科思创德国股份有限公司 | Ionic hydrophilic polyisocyanates and antioxidant |
| EP3666810A1 (en) | 2018-12-13 | 2020-06-17 | Evonik Operations GmbH | Low water content hydrophilic agent and its use in aqueous solutions |
| EP4134386A1 (en) | 2021-08-13 | 2023-02-15 | Evonik Operations GmbH | Adduct compositions made of diisocyanates and hydroxy- or amino-functionalized alkylsulfonic acids and / or alkylsulfonic acid derivatives |
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| CN107082860A (en) * | 2017-04-25 | 2017-08-22 | 周建明 | Self-emulsifying waterborne polyurethane curing agent and preparation method thereof |
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| CN107778447A (en) * | 2017-11-13 | 2018-03-09 | 广东聚盈化工有限公司 | A kind of aqueous one-component moisture polyurethane curing agent and preparation method thereof |
| JP2019189866A (en) * | 2018-04-25 | 2019-10-31 | コベストロ、ドイチュラント、アクチエンゲゼルシャフトＣｏｖｅｓｔｒｏ Ｄｅｕｔｓｃｈｌａｎｄ Ａｇ | Ionically hydrophilized polyisocyanates and radical scavengers and/or peroxide decomposers |
| CN110396173A (en) * | 2018-04-25 | 2019-11-01 | 科思创德国股份有限公司 | Ionic hydrophilic polyisocyanates and free radical scavenger and/or peroxide decomposer |
| CN110396165A (en) * | 2018-04-25 | 2019-11-01 | 科思创德国股份有限公司 | Ionic hydrophilic polyisocyanates and antioxidant |
| JP2019214701A (en) * | 2018-04-25 | 2019-12-19 | コベストロ、ドイチュラント、アクチエンゲゼルシャフトＣｏｖｅｓｔｒｏ Ｄｅｕｔｓｃｈｌａｎｄ Ａｇ | Ionically hydrophilized polyisocyanates and antioxidants |
| EP3666810A1 (en) | 2018-12-13 | 2020-06-17 | Evonik Operations GmbH | Low water content hydrophilic agent and its use in aqueous solutions |
| CN109897160A (en) * | 2019-01-10 | 2019-06-18 | 襄阳精信汇明科技股份有限公司 | Blocked polyurethane curing agent emulsion and preparation method and application thereof |
| CN109897160B (en) * | 2019-01-10 | 2021-02-26 | 襄阳精信汇明科技股份有限公司 | Blocked polyurethane curing agent emulsion and preparation method and application thereof |
| EP4134386A1 (en) | 2021-08-13 | 2023-02-15 | Evonik Operations GmbH | Adduct compositions made of diisocyanates and hydroxy- or amino-functionalized alkylsulfonic acids and / or alkylsulfonic acid derivatives |
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