CN112694593A - Production method of polyurethane resin - Google Patents
Production method of polyurethane resin Download PDFInfo
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- CN112694593A CN112694593A CN202110048809.1A CN202110048809A CN112694593A CN 112694593 A CN112694593 A CN 112694593A CN 202110048809 A CN202110048809 A CN 202110048809A CN 112694593 A CN112694593 A CN 112694593A
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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
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
- C08G18/6677—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203 having at least three hydroxy 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
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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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
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3225—Polyamines
- C08G18/3228—Polyamines acyclic
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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
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
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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
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
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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
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6681—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6685—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
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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
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/6692—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/34
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a production method of polyurethane resin, which comprises the steps of firstly weighing polyethylene glycol, isophorone diisocyanate and toluene diisocyanate in proportion, adding the polyethylene glycol, the isophorone diisocyanate and the toluene diisocyanate into a reaction kettle, heating to 70-90 ℃, stirring for 3-5h at the speed of 100-. By adopting the production method designed by the invention, the use of a large amount of organic solvents can be avoided, the production method is environment-friendly and safe, the overall production time is short, the overall efficiency of the process production can be effectively improved, and the prepared waterborne polyurethane resin has good high-temperature resistance and low-temperature resistance and can ensure good waterproof, corrosion-resistant and wear-resistant performances under extreme environments.
Description
Technical Field
The invention relates to the technical field of polyurethane resin, in particular to a production method of polyurethane resin.
Background
Polyurethane is a polymer composed of organic units connected by urethane, most of polyurethane is thermosetting polymer and can not be melted when being heated, but the polyurethane has thermoplasticity, and with the increasing maturity of the application technology of aqueous resin, a road is paved for the continuous development of the synthetic leather industry, and the popularization and application of the aqueous finishing agent is the inevitable trend of the development of the synthetic leather.
Disclosure of Invention
The invention aims to provide a production method of polyurethane resin, which has the advantage of high efficiency and solves the problem of low efficiency of the existing production method.
In order to achieve the purpose, the invention provides the following technical scheme: the formula of the polyurethane resin comprises the following components in parts by weight:
30-60 parts of polyethylene glycol
20-40 parts of isophorone diisocyanate
15-30 parts of toluene diisocyanate
10-20 parts of dimethylethanolamine
1-3 parts of chain extender
1-2 parts of diluent
1-5 parts of an emulsifier;
a production method of a polyurethane resin, comprising the steps of:
s1, firstly weighing polyethylene glycol, isophorone diisocyanate and toluene diisocyanate in proportion, adding the mixture into a reaction kettle, heating to 70-90 ℃, and stirring for 3-5h at the speed of 100-200r/min to obtain a mixture A for later use;
s2, adding a chain extender into the mixture A, continuously heating to 90-120 ℃, and stirring for 2-4h at the speed of 150-260r/min to obtain a mixture B for later use;
s3, adding a diluent into the mixture B for dilution, adding dimethylethanolamine for neutralization after dilution, keeping the temperature of the reaction kettle at 80-120 ℃ during neutralization and the reaction time at 1-15h, obtaining a mixture C after neutralization, transferring the mixture C into a dispersion tank for dispersion, and stirring after dispersion to obtain a mixture D for later use;
s4, filtering the mixture D to obtain a filtrate, adding an emulsifier into the filtrate, and stirring at a high speed to obtain the polyurethane resin.
Preferably, the chain extender is ethylenediamine, and dimethylolpropionic acid or trimethylolpropane is added when the chain extender is added.
Preferably, the diluent is any one or a mixture of acetone, methyl ethyl ketone, cyclohexanone, benzene, toluene, xylene, n-butanol and styrene.
Preferably, the emulsifier is one or a mixture of more of ethylene glycol butyl ether, methyl acrylate or butyl acrylate.
Preferably, in the fourth step, suspended matters and colloidal impurities in the mixture D are filtered during the filtering, and then soluble salts, colloids, organic matters and microorganisms in the mixture D are filtered by using a reverse osmosis membrane.
Compared with the prior art, the invention has the following beneficial effects:
by adopting the production method designed by the invention, the use of a large amount of organic solvents can be avoided, the production method is environment-friendly and safe, the overall production time is short, the overall efficiency of the process production can be effectively improved, and the prepared waterborne polyurethane resin has good high-temperature resistance and low-temperature resistance and can ensure good waterproof, corrosion-resistant and wear-resistant performances under extreme environments.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme that:
the formula of the polyurethane resin comprises the following components in parts by weight:
30-60 parts of polyethylene glycol
20-40 parts of isophorone diisocyanate
15-30 parts of toluene diisocyanate
10-20 parts of dimethylethanolamine
1-3 parts of chain extender
1-2 parts of diluent
1-5 parts of an emulsifier;
a production method of a polyurethane resin, comprising the steps of:
s1, firstly weighing polyethylene glycol, isophorone diisocyanate and toluene diisocyanate in proportion, adding the mixture into a reaction kettle, heating to 70-90 ℃, and stirring for 3-5h at the speed of 100-200r/min to obtain a mixture A for later use;
s2, adding a chain extender into the mixture A, continuously heating to 90-120 ℃, and stirring for 2-4h at the speed of 150-260r/min to obtain a mixture B for later use;
s3, adding a diluent into the mixture B for dilution, adding dimethylethanolamine for neutralization after dilution, keeping the temperature of the reaction kettle at 80-120 ℃ during neutralization and the reaction time at 1-15h, obtaining a mixture C after neutralization, transferring the mixture C into a dispersion tank for dispersion, and stirring after dispersion to obtain a mixture D for later use;
s4, filtering the mixture D to obtain a filtrate, adding an emulsifier into the filtrate, and stirring at a high speed to obtain the polyurethane resin.
The first embodiment is as follows:
firstly, weighing polyethylene glycol, isophorone diisocyanate and toluene diisocyanate in proportion, adding the polyethylene glycol, isophorone diisocyanate and toluene diisocyanate into a reaction kettle, heating the mixture to 70-90 ℃, stirring the mixture for 3-5 hours at 200r/min for standby, adding a chain extender into the mixture A, continuing heating the mixture to 90-120 ℃, stirring the mixture for 2-4 hours at 260r/min for 150 ℃ for standby, obtaining a mixture B for standby, adding a diluent into the mixture B for dilution, adding dimethylethanolamine for neutralization reaction after the dilution is completed, keeping the reaction kettle at 80-120 ℃ during the neutralization reaction for 1-15 hours, obtaining a mixture C after the neutralization reaction is completed, transferring the mixture C into a dispersion tank for dispersion, stirring the mixture D after the dispersion is completed for standby, and then filtering the mixture D to obtain filtrate, adding an emulsifier into the filtrate, and stirring at a high speed to finally obtain the polyurethane resin.
Example two:
in the first embodiment, the following steps are added:
the chain extender is ethylenediamine, and dimethylolpropionic acid or trimethylolpropane is required to be added when the chain extender is added.
Firstly, weighing polyethylene glycol, isophorone diisocyanate and toluene diisocyanate in proportion, adding the polyethylene glycol, isophorone diisocyanate and toluene diisocyanate into a reaction kettle, heating the mixture to 70-90 ℃, stirring the mixture for 3-5 hours at 200r/min for standby, adding a chain extender into the mixture A, continuing heating the mixture to 90-120 ℃, stirring the mixture for 2-4 hours at 260r/min for 150 ℃ for standby, obtaining a mixture B for standby, adding a diluent into the mixture B for dilution, adding dimethylethanolamine for neutralization reaction after the dilution is completed, keeping the reaction kettle at 80-120 ℃ during the neutralization reaction for 1-15 hours, obtaining a mixture C after the neutralization reaction is completed, transferring the mixture C into a dispersion tank for dispersion, stirring the mixture D after the dispersion is completed for standby, and then filtering the mixture D to obtain filtrate, adding an emulsifier into the filtrate, and stirring at a high speed to finally obtain the polyurethane resin.
Example three:
in the second embodiment, the following steps are added:
the diluent is one or a mixture of more of acetone, methyl ethyl ketone, cyclohexanone, benzene, toluene, xylene, n-butanol and styrene.
Firstly, weighing polyethylene glycol, isophorone diisocyanate and toluene diisocyanate in proportion, adding the polyethylene glycol, isophorone diisocyanate and toluene diisocyanate into a reaction kettle, heating the mixture to 70-90 ℃, stirring the mixture for 3-5 hours at 200r/min for standby, adding a chain extender into the mixture A, continuing heating the mixture to 90-120 ℃, stirring the mixture for 2-4 hours at 260r/min for 150 ℃ for standby, obtaining a mixture B for standby, adding a diluent into the mixture B for dilution, adding dimethylethanolamine for neutralization reaction after the dilution is completed, keeping the reaction kettle at 80-120 ℃ during the neutralization reaction for 1-15 hours, obtaining a mixture C after the neutralization reaction is completed, transferring the mixture C into a dispersion tank for dispersion, stirring the mixture D after the dispersion is completed for standby, and then filtering the mixture D to obtain filtrate, adding an emulsifier into the filtrate, and stirring at a high speed to finally obtain the polyurethane resin.
Example four:
in the third embodiment, the following steps are added:
the emulsifier is one or a mixture of more of ethylene glycol butyl ether, methyl acrylate or butyl acrylate.
Firstly, weighing polyethylene glycol, isophorone diisocyanate and toluene diisocyanate in proportion, adding the polyethylene glycol, isophorone diisocyanate and toluene diisocyanate into a reaction kettle, heating the mixture to 70-90 ℃, stirring the mixture for 3-5 hours at 200r/min for standby, adding a chain extender into the mixture A, continuing heating the mixture to 90-120 ℃, stirring the mixture for 2-4 hours at 260r/min for 150 ℃ for standby, obtaining a mixture B for standby, adding a diluent into the mixture B for dilution, adding dimethylethanolamine for neutralization reaction after the dilution is completed, keeping the reaction kettle at 80-120 ℃ during the neutralization reaction for 1-15 hours, obtaining a mixture C after the neutralization reaction is completed, transferring the mixture C into a dispersion tank for dispersion, stirring the mixture D after the dispersion is completed for standby, and then filtering the mixture D to obtain filtrate, adding an emulsifier into the filtrate, and stirring at a high speed to finally obtain the polyurethane resin.
Example five:
in the fourth example, the following steps were added:
in the fourth step, suspended matters and colloid impurities in the mixture D are filtered firstly during filtering, and then soluble salt, colloid, organic matters and microorganisms in the mixture D are filtered by utilizing a reverse osmosis membrane.
Firstly, weighing polyethylene glycol, isophorone diisocyanate and toluene diisocyanate in proportion, adding the polyethylene glycol, isophorone diisocyanate and toluene diisocyanate into a reaction kettle, heating the mixture to 70-90 ℃, stirring the mixture for 3-5 hours at 200r/min for standby, adding a chain extender into the mixture A, continuing heating the mixture to 90-120 ℃, stirring the mixture for 2-4 hours at 260r/min for 150 ℃ for standby, obtaining a mixture B for standby, adding a diluent into the mixture B for dilution, adding dimethylethanolamine for neutralization reaction after the dilution is completed, keeping the reaction kettle at 80-120 ℃ during the neutralization reaction for 1-15 hours, obtaining a mixture C after the neutralization reaction is completed, transferring the mixture C into a dispersion tank for dispersion, stirring the mixture D after the dispersion is completed for standby, and then filtering the mixture D to obtain filtrate, adding an emulsifier into the filtrate, and stirring at a high speed to finally obtain the polyurethane resin.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. The formula of the polyurethane resin is characterized in that: the components of the material comprise the following components in parts by weight:
30-60 parts of polyethylene glycol
20-40 parts of isophorone diisocyanate
15-30 parts of toluene diisocyanate
10-20 parts of dimethylethanolamine
1-3 parts of chain extender
1-2 parts of diluent
1-5 parts of an emulsifier;
a production method of a polyurethane resin, comprising the steps of:
s1, firstly weighing polyethylene glycol, isophorone diisocyanate and toluene diisocyanate in proportion, adding the mixture into a reaction kettle, heating to 70-90 ℃, and stirring for 3-5h at the speed of 100-200r/min to obtain a mixture A for later use;
s2, adding a chain extender into the mixture A, continuously heating to 90-120 ℃, and stirring for 2-4h at the speed of 150-260r/min to obtain a mixture B for later use;
s3, adding a diluent into the mixture B for dilution, adding dimethylethanolamine for neutralization after dilution, keeping the temperature of the reaction kettle at 80-120 ℃ during neutralization and the reaction time at 1-15h, obtaining a mixture C after neutralization, transferring the mixture C into a dispersion tank for dispersion, and stirring after dispersion to obtain a mixture D for later use;
s4, filtering the mixture D to obtain a filtrate, adding an emulsifier into the filtrate, and stirring at a high speed to obtain the polyurethane resin.
2. The production method of a polyurethane resin according to claim 1, characterized in that: the chain extender is ethylenediamine, and dimethylolpropionic acid or trimethylolpropane is required to be added when the chain extender is added.
3. The production method of a polyurethane resin according to claim 1, characterized in that: the diluent is one or a mixture of more of acetone, methyl ethyl ketone, cyclohexanone, benzene, toluene, xylene, n-butanol and styrene.
4. The production method of a polyurethane resin according to claim 1, characterized in that: the emulsifier is one or a mixture of more of ethylene glycol butyl ether, methyl acrylate or butyl acrylate.
5. The production method of a polyurethane resin according to claim 1, characterized in that: in the fourth step, suspended matters and colloid impurities in the mixture D are filtered firstly during filtering, and then soluble salt, colloid, organic matters and microorganisms in the mixture D are filtered by utilizing a reverse osmosis membrane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110048809.1A CN112694593A (en) | 2021-01-14 | 2021-01-14 | Production method of polyurethane resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110048809.1A CN112694593A (en) | 2021-01-14 | 2021-01-14 | Production method of polyurethane resin |
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| CN112694593A true CN112694593A (en) | 2021-04-23 |
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| CN202110048809.1A Pending CN112694593A (en) | 2021-01-14 | 2021-01-14 | Production method of polyurethane resin |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101328383A (en) * | 2008-07-17 | 2008-12-24 | 安徽大学 | Production method for liner gloves aqueous polyurethane coating connection material |
| CN104211898A (en) * | 2014-08-13 | 2014-12-17 | 佛山市顺德区巴德富实业有限公司 | Amino-terminated aqueous polyurethane dispersion and preparation method thereof |
| CN110938185A (en) * | 2018-09-25 | 2020-03-31 | 上海弘业涂料科技发展有限公司 | Preparation method of waterborne polyurethane resin |
-
2021
- 2021-01-14 CN CN202110048809.1A patent/CN112694593A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101328383A (en) * | 2008-07-17 | 2008-12-24 | 安徽大学 | Production method for liner gloves aqueous polyurethane coating connection material |
| CN104211898A (en) * | 2014-08-13 | 2014-12-17 | 佛山市顺德区巴德富实业有限公司 | Amino-terminated aqueous polyurethane dispersion and preparation method thereof |
| CN110938185A (en) * | 2018-09-25 | 2020-03-31 | 上海弘业涂料科技发展有限公司 | Preparation method of waterborne polyurethane resin |
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Application publication date: 20210423 |