CN105732930A - Water-resistant agent and preparation method thereof - Google Patents
Water-resistant agent and preparation method thereof Download PDFInfo
- Publication number
- CN105732930A CN105732930A CN201610277639.3A CN201610277639A CN105732930A CN 105732930 A CN105732930 A CN 105732930A CN 201610277639 A CN201610277639 A CN 201610277639A CN 105732930 A CN105732930 A CN 105732930A
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- CN
- China
- Prior art keywords
- water
- alcohol
- sprinkling agent
- resistant agent
- reaction
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention relates to a synthetic leather auxiliary, in particular relates to a water-resistant agent and a preparation method thereof, and aims to provide a water-resistant agent which is prepared by comprehensively utilizing a mode of polyurethane molecular chain elongation and by using an improved synthesis process and is free of harm or pollution and good in hydrolysis resistance. The water-resistant agent is prepared from the following components: 20-28% of isocyanate, 6-10% of low molecular weight alcohol, 18-28% of halogen alcohol, 5-8% of an amine terminator, 28% of a solvent MEK and 12% of a solvent DMF. The water-resistant agent provided by the invention is prepared by taking non-fusible halogen alcohol as a main water-resistant component by using a polyurethane synthesis method and an improved synthesis process in a mode of polyurethane molecular chain elongation; as halogen alcohol participates in the reaction sufficiently, no monomer residues can be caused in the synthesized water-resistant agent, no harm can be done to human bodies, environment pollution can be reduced, the water-resistant effect of the water-resistant agent can be improved to the maximum extent, and thus the water-resistant agent is a polyurethane resin auxiliary with excellent water resistance.
Description
Technical field
The present invention relates to a kind of synthetic leather auxiliary agent, particularly to a kind of water-sprinkling agent and preparation method thereof.
Background technology
Synthetic leather (such as footwear leather, luggage leather, clothing leather etc.) make after through there will be the phenomenons such as cracking and fragmentation after a while under dampness effect.The existence of moisture in air easily causes hydrolysis, thus shortens synthetic leather service life, and the product of damaged can not use because not reaching high physical property and requiring.
Need to add to improve the problem such as hydrolysis there is the plain alcohols water-sprinkling agent of high water resistance, increase or expand its water-sprinkling effect to greatest extent, strengthen the high hydrolysis resistance performance of synthetic leather, improve physical property, extend product service life.
But, the synthetic leather course of processing is used alone element alcohol analog assistant, its water-sprinkling effect imperfection, there is the adverse effect such as personal injury and environmental hazard.It is thus desirable to research and development are to human body non-hazardous, non-environmental-pollution, the water-sprinkling agent of high hydrolysis resistance performance.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of mode comprehensively utilizing polyurethane molecular chain elongation, improve non-hazardous, pollution-free, the water-sprinkling agent of high hydrolysis resistance performance that synthesis technique prepares.
In order to achieve the above object, a kind of water-sprinkling agent of the present invention, prepared by following component by weight percentage:
Isocyanates: 20%-28%,
Low-molecular-weight alcohol: 6%-10%,
Element alcohol: 18%-28%,
Amine terminator: 5%-8%,
Solvent MEK:28%,
Solvent DMF: 12%;
Described isocyanates is unimolecule structure isocyanates, and described low-molecular-weight alcohol is unimolecule structure alcohol.
As preferably, described isocyanates is toluene di-isocyanate(TDI) TDI and one in methyl diphenylene diisocyanate MDI.
As preferably, described low-molecular-weight alcohol is neopentyl glycol NPG and one in ethylene glycol EG.
As preferably, described element alcohol is fluorine element alcohol.
As preferably, the preparation component of described water-sprinkling agent also includes catalyst EC-305, and consumption is 0.01%, and synthesising reacting speed can be made to accelerate.
It is a further object of the present invention to provide the preparation method of a kind of water-sprinkling agent, comprise the steps: the consumption of all raw materials by weight percentage
Step one: first putting into the isocyanates of 20%-28% in a kettle., the low-molecular-weight alcohol the most in batches putting into 6%-10% reacts, reaction keeps reaction 1 hour after terminating at 60-70 DEG C;Initial reaction stage cools down in time along with the rising of temperature, stablizes temperature of reaction kettle, prevents gelatin phenomenon;
Step 2: put in reactor after being dissolved in the mixed solvent being made up of the MEK of 28% and the DMF of 12% by the plain alcohol of 18%-28%, keeps temperature of reaction kettle at 65-70 DEG C, prevents from feeding intake too fast;
Step 3: synthetic reaction puts into the amine terminator of 7%-8% the most afterwards and terminates synthetic reaction.
As preferably, described isocyanates is toluene di-isocyanate(TDI) TDI and one in methyl diphenylene diisocyanate MDI.
As preferably, described low-molecular-weight alcohol is neopentyl glycol NPG and one in ethylene glycol EG.
As preferably, described element alcohol is fluorine element alcohol.
As preferably, after described step 2 stirs 1 hour after element alcohol adds, add the catalyst EC-305 of 0.01%.
The water-sprinkling agent of the present invention is to be main water-sprinkling composition with non-fusibility element alcohols, uses the synthetic method of polyurethane, the mode of comprehensive utilization polyurethane molecular chain elongation, improves synthesis technique and prepare;Owing to element alcohol fully participates in reaction, in the water-sprinkling agent of synthesis, there is no monomer residue, to human body non-hazardous, reduce environmental pollution, increase or expand its water-sprinkling effect to greatest extent, be the polyurethane resin auxiliary agent of a kind of water repellency excellence.
Detailed description of the invention
Embodiment
1
:
A kind of water-sprinkling agent, is prepared by following component:
Unimolecule structure toluene di-isocyanate(TDI) TDI:244.20g
Unimolecule structure neopentyl glycol NPG:73.00g
Fluorine element alcohol: 210.00g
Amine terminator: 72.70g
Solvent MEK:280.00g
Solvent DMF: 120.00g
Catalyst EC-305:0.10g
The preparation method of above-mentioned water-sprinkling agent is as follows:
Step one: put into 244.20g unimolecule structure toluene di-isocyanate(TDI) TDI the most in a kettle., puts into 73.00g unimolecule structure neopentyl glycol NPG the most in batches and reacts, and reaction keeps reaction 1 hour after terminating at 60-70 DEG C;Initial reaction stage cools down in time along with the rising of temperature, stablizes temperature of reaction kettle, prevents gelatin phenomenon;
Step 2: put in reactor after 210.00g fluorine element alcohol is dissolved in the mixed solvent being made up of 280.00g MEK and 120.00gDMF, stir 1 hour after fluorine element alcohol adds, it is subsequently adding 0.10g catalyst EC-305, keeps temperature of reaction kettle at 65-70 DEG C, prevent from feeding intake too fast;
Step 3: synthetic reaction puts into 72.70g amine terminator the most afterwards and terminates synthetic reaction.
Testing the transparency of above-mentioned water-sprinkling agent, water-sprinkling degree, synthesising stability and processing stability, test result see table:
Embodiment
2
:
A kind of water-sprinkling agent, is prepared by following component:
Unimolecule structure methyl diphenylene diisocyanate MDI:268.20g
Unimolecule structure neopentyl glycol NPG:62.70g
Fluorine element alcohol: 210.00g
Amine terminator: 59.00g
Solvent MEK:280.00g
Solvent DMF: 120.00g
Catalyst EC-305:0.10g
The preparation method of above-mentioned water-sprinkling agent is as follows:
Step one: put into 268.20g unimolecule structure methyl diphenylene diisocyanate MDI the most in a kettle., puts into 62.70g unimolecule structure neopentyl glycol NPG the most in batches and reacts, and reaction keeps reaction 1 hour after terminating at 60-70 DEG C;Initial reaction stage cools down in time along with the rising of temperature, stablizes temperature of reaction kettle, prevents gelatin phenomenon;
Step 2: put in reactor after 210.00g fluorine element alcohol is dissolved in the mixed solvent being made up of 280.00g MEK and 120.00gDMF, stir 1 hour after fluorine element alcohol adds, it is subsequently adding 0.10g catalyst EC-305, keeps temperature of reaction kettle at 65-70 DEG C, prevent from feeding intake too fast;
Step 3: synthetic reaction puts into 59.00g amine terminator the most afterwards and terminates synthetic reaction.
Testing the transparency of above-mentioned water-sprinkling agent, water-sprinkling degree, synthesising stability and processing stability, test result see table:
Embodiment
3
:
A kind of water-sprinkling agent, is prepared by following component:
Unimolecule structure toluene di-isocyanate(TDI) TDI:238.90g
Unimolecule structure ethylene glycol EG:81.00g
Fluorine element alcohol: 210.00g
Amine terminator: 70.00g
Solvent MEK:280.00g
Solvent DMF: 120.00g
Catalyst EC-305:0.10g
The preparation method of above-mentioned water-sprinkling agent is as follows:
Step one: put into 238.90g unimolecule structure toluene di-isocyanate(TDI) TDI the most in a kettle., puts into 81.00g unimolecule structure ethylene glycol EG the most in batches and reacts, and reaction keeps reaction 1 hour after terminating at 60-70 DEG C;Initial reaction stage cools down in time along with the rising of temperature, stablizes temperature of reaction kettle, prevents gelatin phenomenon;
Step 2: put in reactor after 210.00g fluorine element alcohol is dissolved in the mixed solvent being made up of 280.00g MEK and 120.00gDMF, stir 1 hour after fluorine element alcohol adds, it is subsequently adding 0.10g catalyst EC-305, keeps temperature of reaction kettle at 65-70 DEG C, prevent from feeding intake too fast;
Step 3: synthetic reaction puts into 70.00g amine terminator the most afterwards and terminates synthetic reaction.
Testing the transparency of above-mentioned water-sprinkling agent, water-sprinkling degree, synthesising stability and processing stability, test result see table:
Claims (10)
1. a water-sprinkling agent, it is characterised in that: prepared by following component by weight percentage:
Isocyanates: 20%-28%,
Low-molecular-weight alcohol: 6%-10%,
Element alcohol: 18%-28%,
Amine terminator: 5%-8%,
Solvent MEK:28%,
Solvent DMF: 12%;
Described isocyanates is unimolecule structure isocyanates, and described low-molecular-weight alcohol is unimolecule structure alcohol.
A kind of water-sprinkling agent the most according to claim 1, it is characterised in that: described isocyanates is toluene di-isocyanate(TDI) TDI and one in methyl diphenylene diisocyanate MDI.
A kind of water-sprinkling agent the most according to claim 1 and 2, it is characterised in that: described low-molecular-weight alcohol is neopentyl glycol NPG and one in ethylene glycol EG.
A kind of water-sprinkling agent the most according to claim 1 and 2, it is characterised in that: described element alcohol is fluorine element alcohol.
A kind of water-sprinkling agent the most according to claim 3, it is characterised in that: described element alcohol is fluorine element alcohol.
A kind of water-sprinkling agent the most according to claim 1, it is characterised in that: the preparation component of described water-sprinkling agent also includes the catalyst EC-305 of 0.01%.
7. a preparation method for water-sprinkling agent, comprises the steps: the consumption of all raw materials by weight percentage
Step one: first putting into the unimolecule structure isocyanates of 20%-28% in a kettle., the unimolecule structure low-molecular-weight alcohol the most in batches putting into 6%-10% reacts, reaction keeps reaction 1 hour after terminating at 60-70 DEG C;Initial reaction stage cools down in time along with the rising of temperature, stablizes temperature of reaction kettle, prevents gelatin phenomenon;
Step 2: put in reactor after being dissolved in the mixed solvent being made up of the MEK of 28% and the DMF of 12% by the plain alcohol of 18%-28%, keeps temperature of reaction kettle at 65-70 DEG C, prevents from feeding intake too fast;
Step 3: synthetic reaction puts into the amine terminator of 7%-8% the most afterwards and terminates synthetic reaction.
The preparation method of a kind of water-sprinkling agent the most according to claim 7, it is characterized in that: described unimolecule structure isocyanates is toluene di-isocyanate(TDI) TDI and one in methyl diphenylene diisocyanate MDI, described unimolecule structure low-molecular-weight alcohol is neopentyl glycol NPG and one in ethylene glycol EG.
9. according to the preparation method of a kind of water-sprinkling agent described in claim 7 or 8, it is characterised in that: described element alcohol is fluorine element alcohol.
The preparation method of a kind of water-sprinkling agent the most according to claim 7, it is characterised in that: add the catalyst EC-305 of 0.01% after described step 2 stirs 1 hour after element alcohol adds.
Priority Applications (1)
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CN201610277639.3A CN105732930A (en) | 2016-04-29 | 2016-04-29 | Water-resistant agent and preparation method thereof |
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CN201610277639.3A CN105732930A (en) | 2016-04-29 | 2016-04-29 | Water-resistant agent and preparation method thereof |
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CN201610277639.3A Pending CN105732930A (en) | 2016-04-29 | 2016-04-29 | Water-resistant agent and preparation method thereof |
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1661158A (en) * | 2004-02-24 | 2005-08-31 | 福盈科技化学股份有限公司 | Hydrophobic and oleophobic agent in fluoric solvent type and producing method |
CN101979756A (en) * | 2010-09-20 | 2011-02-23 | 上海汇得化工有限公司 | Drying agent for polyurethane synthetic leather and preparation method thereof |
CN102417575A (en) * | 2011-11-01 | 2012-04-18 | 吴江市北厍盛源纺织品助剂厂 | Preparation method of fluorine-containing aqueous polyurethane water-repellent oil-repellent finishing agent |
-
2016
- 2016-04-29 CN CN201610277639.3A patent/CN105732930A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1661158A (en) * | 2004-02-24 | 2005-08-31 | 福盈科技化学股份有限公司 | Hydrophobic and oleophobic agent in fluoric solvent type and producing method |
CN101979756A (en) * | 2010-09-20 | 2011-02-23 | 上海汇得化工有限公司 | Drying agent for polyurethane synthetic leather and preparation method thereof |
CN102417575A (en) * | 2011-11-01 | 2012-04-18 | 吴江市北厍盛源纺织品助剂厂 | Preparation method of fluorine-containing aqueous polyurethane water-repellent oil-repellent finishing agent |
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Application publication date: 20160706 |