CN103951809A - Preparation method of polyurethane modified organic silicon multipolymer fabric softening agent - Google Patents
Preparation method of polyurethane modified organic silicon multipolymer fabric softening agent Download PDFInfo
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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
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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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
- C08G18/70—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
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- 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
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
- C08G77/16—Polysiloxanes containing silicon bound to oxygen-containing groups to hydroxyl groups
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- 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
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/653—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain modified by isocyanate compounds
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- 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
- D06M2200/50—Modified hand or grip properties; Softening compositions
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- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a preparation method of a polyurethane modified organic silicon multipolymer fabric softening agent. The preparation method comprises the following steps: firstly preparing a polyurethane prepolymer by using polyethylene glycol 2000 and isophorone diisocyanate; then preparing alkylhydroxyl-containing silicone oil by using di-n-butyl amine, epoxy 1,3-bis(3-glycidoxypropyl)-1,1,3,3-tetramethyldisiloxane and octamethyl cyclotetrasiloxane; reacting the polyurethane prepolymer with the alkylhydroxyl-containing silicone oil so as to obtain a polyurethane organic silicon multipolymer; and finally adding deionized water, and emulsifying so as to obtain the polyurethane modified organic silicon multipolymer fabric softening agent. The preparation method of the polyurethane modified organic silicon multipolymer fabric softening agent has the beneficial effects that urethane groups and urethane are introduced into organic silicon and serve as hard chain segments for generation of physical crosslinking, meanwhile, polyether is introduced and serves as a hydrophilic chain segment, the problem that as an amino silicon oil softening agent is easy to yellow and demulsify, oil patches are formed on fabrics, is solved, the hydrophilic performance of the fabrics subjected to soft finish is improved, the wearing hygroscopicity of the fabrics is improved, and the durability of the fabrics is good.
Description
Technical field
The invention belongs to the preparing technical field of textiles auxiliary agent, be specifically related to a kind of preparation method of polyurethane-modified organosilicon multiple copolymer fabric softener.
Background technology
Polydimethylsiloxane is the fabric softener that a kind of performance is very superior, due to its good molecular flexibility and abundant methyl content, can be so that form methyl tectum at fiber surface, thus the static and dynamic friction coefficient between fiber reduced, reach good soft effect.But because it does not firmly form bonding force with fiber, just by a limited number of Van der Waals forces and hydrogen bond, be combined with fiber, meanwhile, so owing to not having the crosslinkable group cannot be separately in fiber surface film forming in molecule, fastness be poor.In order to address these problems, people have developed the organosilicon product of many improvement, wherein take amido silicon oil as representative, due to amino existence, under solutions of weak acidity, amino can cationization, generation can form the comparatively firmly bonding that electrostatic attraction is combined by negative charge group on fiber, fastness is better than common silicone oil, and the effect due to this electrostatic attraction, having made the more methyl can be outside, so series products has the effect of super softness, be the best organosilicon product of softness in the market.But amino silicon also has its shortcoming, because the nitrogen-atoms cloud density in amino is higher, so easy and absorb light electronics generation photochemical reaction, thereby produce so-called Yellowing, and amido silicon oil is difficult for emulsification in addition, easily breakdown of emulsion forms the poor shortcoming of the wetting abilities such as oil mark on fabric.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of polyurethane-modified organosilicon multiple copolymer fabric softener, solved that amino-silicone oil softening agent easily produces Yellowing, easily breakdown of emulsion forms the problem of oil mark on fabric.
The technical solution adopted in the present invention is: a kind of preparation method of polyurethane-modified organosilicon multiple copolymer fabric softener, specifically comprises the following steps:
Step 1: prepare base polyurethane prepolymer for use as
Macrogol 2000 is carried out to vacuum-drying, after vacuum-drying, lower the temperature, the Macrogol 2000 through vacuum-drying cooling is added in flask, and add isophorone diisocyanate and catalyzer in flask, then be warming up to 60～80 ℃, reaction 1～4h, obtains base polyurethane prepolymer for use as;
Step 2: prepare alkane hydroxy silicon oil
In flask, add Di-n-Butyl Amine and epoxy double-seal head according to a certain percentage, be warming up to 60～100 ℃ of reaction 2～6h; Then to the octamethylcyclotetrasiloxane and the catalyzer that add certain mass in flask, be warming up to 110～130 ℃ of reaction 1～4h, obtain alkane hydroxy silicon oil;
Step 3: prepare urethane organosilicon multiple copolymer
The alkane hydroxy silicon oil that the base polyurethane prepolymer for use as that step 1 is obtained and step 2 obtain adds in flask according to a certain percentage, is then warming up to 50～80 ℃ of reaction 1～4h, obtains urethane organosilicon multiple copolymer;
Step 4: prepare polyurethane-modified organosilicon multiple copolymer fabric softener
In the organosilicon multiple copolymer obtaining to step 3, add deionized water to be diluted to the solid content of needs, stirring and emulsifying, obtains.
Feature of the present invention is also,
In step 1, vacuum drying temperature is 110～120 ℃, vacuum tightness 0.08～0.09MPa, and the time is 2～4h, is cooled to 45～50 ℃ after vacuum-drying.
In step 1, the mol ratio of isophorone diisocyanate and Macrogol 2000 is 1.2～1.8:1.
In step 1, catalyzer is dibutyl tin dilaurate, and consumption is 1/2000～1/1000 of Macrogol 2000 and isophorone diisocyanate quality summation.
In step 2, the mol ratio of Di-n-Butyl Amine and epoxy double-seal head is 1:1.
In step 2, the mass ratio of octamethylcyclotetrasiloxane and epoxy double-seal head is 5～20:1.
In step 2, catalyzer is Tetramethylammonium hydroxide, and the quality of catalyzer is with respect to 1/1000 of octamethylcyclotetrasiloxane quality.
In step 3, the mol ratio of base polyurethane prepolymer for use as and alkane hydroxy silicon oil is 1:1.
In step 3, add catalyzer dibutyl tin dilaurate, the quality of dibutyl tin dilaurate is 1/2000～1/1000 of base polyurethane prepolymer for use as and alkane hydroxy silicon oil quality summation.
In step 4, churning time is 2～4h.
The invention has the beneficial effects as follows: the preparation method of a kind of polyurethane-modified organosilicon multiple copolymer fabric softener of the present invention, in organosilicon, introduce urea ester group and urethano as the hard segment that produces physical crosslinking, introduce polyethers as hydrophilic segment simultaneously, solved that amino-silicone oil softening agent easily produces Yellowing, easily breakdown of emulsion forms the problem of oil mark on fabric, improved the hydrophilicity after fabric sofetening arranges, improved and worn water absorbability and good endurance.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
The preparation method of a kind of polyurethane-modified organosilicon multiple copolymer fabric softener of the present invention, specifically comprises the following steps: specifically comprise the following steps:
Step 1: prepare base polyurethane prepolymer for use as
Macrogol 2000 (PEG2000) is carried out to vacuum-drying, vacuum drying temperature is 110～120 ℃, vacuum tightness 0.08～0.09MPa, time is 2～4h, after vacuum-drying, be cooled to 45～50 ℃, PEG2000 through vacuum-drying cooling is added in flask, and add isophorone diisocyanate (IPDI) and catalyzer dibutyl tin dilaurate in flask, the mol ratio of IPDI and PEG2000 is 1.2～1.8:1, dibutyl tin dilaurate consumption is 1/2000～1/1000 of PEG2000 and IPDI quality summation, then be warming up to 60～80 ℃, reaction 1～4h, obtain base polyurethane prepolymer for use as,
Step 2: prepare alkane hydroxy silicon oil
According to mol ratio, be that 1:1 adds Di-n-Butyl Amine and epoxy double-seal head in flask, be warming up to 60～100 ℃ of reaction 2～6h; Then to the octamethylcyclotetrasiloxane (D that adds certain mass in flask
4) and catalyzer Tetramethylammonium hydroxide, D
4with the mass ratio of epoxy double-seal head be 5～20:1, the quality of Tetramethylammonium hydroxide is with respect to D
41/1000 of quality, is warming up to 110～130 ℃ of reaction 1～4h, obtains alkane hydroxy silicon oil;
Step 3: prepare urethane organosilicon multiple copolymer
The alkane hydroxy silicon oil that the base polyurethane prepolymer for use as that step 1 is obtained and step 2 obtain adds in flask according to mol ratio 1:1, is then warming up to 50～80 ℃ of reaction 1～4h, obtains urethane organosilicon multiple copolymer; For Reaction time shorten, can add 1/2000～1/1000 catalyzer dibutyl tin dilaurate of base polyurethane prepolymer for use as and alkane hydroxy silicon oil quality summation;
Step 4: prepare polyurethane-modified organosilicon multiple copolymer fabric softener
In the organosilicon multiple copolymer obtaining to step 3, add deionized water to be diluted to the solid content of needs, stirring and emulsifying 2～4h, obtains.
Solid content (%)=m (organosilicon multiple copolymer)/m (organosilicon multiple copolymer+deionized water) * 100%.
The preparation method of a kind of polyurethane-modified organosilicon multiple copolymer fabric softener of the present invention, introduce vulcabond as comonomer, in organosilicon, introduce urea ester group and urethano as the hard segment that produces physical crosslinking, introduce polyethers simultaneously and strengthen organosilyl wetting ability as hydrophilic segment; Utilize " positioning action " upper ammonia ester bond and urea ester bond to improve silicone softening agent oriented adsorption and durability degree; Adopt isolation group that Si～O～C key is kept apart and improved the organosilyl hydrolytic resistance of urethane; And retain end group isocyano as crosslinked group.
Beneficial effect of the present invention: make that polyurethane-modified organosilicon multiple copolymer fabric softener hydrophilicity is good, storage properties is stable, emulsification is simple, emulsion property is stablized and hydrolysis, apply it in fabric sofetening arrangement and first can promote the softness of fabric, comprise raising smoothness, reduce static and dynamic friction coefficient; There is not remarkable decline in the fabric hydrophilic after arrangement; Physical point of attachment in molecular structure is abundant, can strengthen its " positioning action " and promote soft durability degree; In use procedure, not needing additionally to add emulsifying agent emulsification, also there is no emulsifying agent in product emulsion, is a kind of complete self-emulsifying product, meets the trend of current environmental protection; Use procedure is simple, and product emulsion is directly opened and rarely just can be used, and operation bidirectional, can not improve large production efficiency.
Embodiment 1
Step 1: prepare base polyurethane prepolymer for use as
PEG2000 is carried out to vacuum-drying, vacuum drying temperature is 120 ℃, vacuum tightness 0.08MPa, the time is 2h, is cooled to 50 ℃ after vacuum-drying, the PEG2000 that gets 50g process vacuum-drying cooling adds in flask, and add 10g IPDI (mol ratio of IPDI and PEG2000 is 1.8:1) and 0.03g catalyzer dibutyl tin dilaurate in flask, be then warming up to 70 ℃, reaction 3h, reaction finishes rear cooling, obtains base polyurethane prepolymer for use as;
Step 2: prepare alkane hydroxy silicon oil
According to mol ratio, be that 1:1 adds 6.4g Di-n-Butyl Amine and 9g epoxy double-seal head in flask, be warming up to 80 ℃ of reaction 4h; Then to the D that adds 90g in flask
4(D
4with the mass ratio of epoxy double-seal head be 10:1) and 0.09g catalyzer Tetramethylammonium hydroxide, be warming up to 120 ℃ of reaction 3h, reaction finishes rear cooling, obtains alkane hydroxy silicon oil;
Step 3: prepare urethane organosilicon multiple copolymer
The alkane hydroxy silicon oil that the base polyurethane prepolymer for use as that step 1 is obtained and step 2 obtain adds in flask according to mol ratio 1:1, the catalyzer dibutyl tin dilaurate that simultaneously adds base polyurethane prepolymer for use as and alkane hydroxy silicon oil quality summation 1/1250, then be warming up to 70 ℃ of reaction 2h, reaction finishes rear cooling, obtains urethane organosilicon multiple copolymer;
Step 4: prepare polyurethane-modified organosilicon multiple copolymer fabric softener
In the organosilicon multiple copolymer obtaining to step 3, add deionized water to be diluted to 30% solid content, stirring and emulsifying 2h, obtains.
Embodiment 2
Step 1: prepare base polyurethane prepolymer for use as
PEG2000 is carried out to vacuum-drying, vacuum drying temperature is 110 ℃, vacuum tightness 0.09MPa, the time is 4h, is cooled to 50 ℃ after vacuum-drying, the PEG2000 that gets 50g process vacuum-drying cooling adds in flask, and add 6.666g IPDI (mol ratio of IPDI and PEG2000 is 1.2:1) and 0.0453g catalyzer dibutyl tin dilaurate in flask, be then warming up to 60 ℃, reaction 4h, reaction finishes rear cooling, obtains base polyurethane prepolymer for use as;
Step 2: prepare alkane hydroxy silicon oil
According to mol ratio, be that 1:1 adds 6.4g Di-n-Butyl Amine and 9g epoxy double-seal head in flask, be warming up to 60 ℃ of reaction 6h; Then to the D that adds 45g in flask
4(D
4with the mass ratio of epoxy double-seal head be 5:1) and 0.005g catalyzer Tetramethylammonium hydroxide, be warming up to 110 ℃ of reaction 4h, reaction finishes rear cooling, obtains alkane hydroxy silicon oil;
Step 3: prepare urethane organosilicon multiple copolymer
The alkane hydroxy silicon oil that the base polyurethane prepolymer for use as that step 1 is obtained and step 2 obtain adds in flask according to mol ratio 1:1,1/1000 the catalyzer dibutyl tin dilaurate that simultaneously adds base polyurethane prepolymer for use as and alkane hydroxy silicon oil quality summation, then be warming up to 60 ℃ of reaction 3h, reaction finishes rear cooling, obtains urethane organosilicon multiple copolymer;
Step 4: prepare polyurethane-modified organosilicon multiple copolymer fabric softener
In the organosilicon multiple copolymer obtaining to step 3, add deionized water to be diluted to 20% solid content, stirring and emulsifying 3h, obtains.
Embodiment 3
Step 1: prepare base polyurethane prepolymer for use as
PEG2000 is carried out to vacuum-drying, vacuum drying temperature is 115 ℃, vacuum tightness 0.09MPa, the time is 3h, is cooled to 45 ℃ after vacuum-drying, the PEG2000 that gets 50g process vacuum-drying cooling adds in flask, and add 8.333g IPDI (mol ratio of IPDI and PEG2000 is 1.5:1) and 0.0467g catalyzer dibutyl tin dilaurate in flask, be then warming up to 80 ℃, reaction 1h, reaction finishes rear cooling, obtains base polyurethane prepolymer for use as;
Step 2: prepare alkane hydroxy silicon oil
According to mol ratio, be that 1:1 adds 6.4g Di-n-Butyl Amine and 9g epoxy double-seal head in flask, be warming up to 100 ℃ of reaction 2h; Then to the D that adds 180g in flask
4(D
4with the mass ratio of epoxy double-seal head be 20:1) and 0.18g catalyzer Tetramethylammonium hydroxide, be warming up to 130 ℃ of reaction 1h, reaction finishes rear cooling, obtains alkane hydroxy silicon oil;
Step 3: prepare urethane organosilicon multiple copolymer
The alkane hydroxy silicon oil that the base polyurethane prepolymer for use as that step 1 is obtained and step 2 obtain adds in flask according to mol ratio 1:1, is then warming up to 80 ℃ of reaction 1h, and reaction finishes rear cooling, obtains urethane organosilicon multiple copolymer;
Step 4: prepare polyurethane-modified organosilicon multiple copolymer fabric softener
In the organosilicon multiple copolymer obtaining to step 3, add deionized water to be diluted to 10% solid content, stirring and emulsifying 4h, obtains.
Embodiment 4
Step 1: prepare base polyurethane prepolymer for use as
PEG2000 is carried out to vacuum-drying, vacuum drying temperature is 120 ℃, vacuum tightness 0.085MPa, the time is 2h, is cooled to 48 ℃ after vacuum-drying, the PEG2000 that gets 50g process vacuum-drying cooling adds in flask, and add 7.7778g IPDI (mol ratio of IPDI and PEG2000 is 1.4:1) and 0.0577g catalyzer dibutyl tin dilaurate in flask, be then warming up to 70 ℃, reaction 2h, reaction finishes rear cooling, obtains base polyurethane prepolymer for use as;
Step 2: prepare alkane hydroxy silicon oil
According to mol ratio, be that 1:1 adds 6.4g Di-n-Butyl Amine and 9g epoxy double-seal head in flask, be warming up to 90 ℃ of reaction 2h; Then to the D that adds 135g in flask
4(D
4with the mass ratio of epoxy double-seal head be 15:1) and 0.135g catalyzer Tetramethylammonium hydroxide, be warming up to 120 ℃ of reaction 3h, reaction finishes rear cooling, obtains alkane hydroxy silicon oil;
Step 3: prepare urethane organosilicon multiple copolymer
The alkane hydroxy silicon oil that the base polyurethane prepolymer for use as that step 1 is obtained and step 2 obtain adds in flask according to mol ratio 1:1, the catalyzer dibutyl tin dilaurate that simultaneously adds base polyurethane prepolymer for use as and alkane hydroxy silicon oil quality summation 1/2000, then be warming up to 50 ℃ of reaction 4h, reaction finishes rear cooling, obtains urethane organosilicon multiple copolymer;
Step 4: prepare polyurethane-modified organosilicon multiple copolymer fabric softener
In the organosilicon multiple copolymer obtaining to step 3, add deionized water to be diluted to 15% solid content, stirring and emulsifying 2h, obtains.
The effect comparison that table 1 fabric softener of the present invention and amido silicon oil arrange fabric sofetening
From the data of table 1, can find out, the present invention is more or less the same with commercially available amido silicon oil on soft effect, and can produce the feel more more smooth than amido silicon oil, the time of oozing under water droplet is shorter, show that wetting ability is better, fabric softener of the present invention affects the hydrophilicity of fabric hardly, and wetting ability is far superior to the fabric that amido silicon oil is processed.
Claims (10)
1. a preparation method for polyurethane-modified organosilicon multiple copolymer fabric softener, is characterized in that, specifically comprises the following steps:
Step 1: prepare base polyurethane prepolymer for use as
Macrogol 2000 is carried out to vacuum-drying, after vacuum-drying, lower the temperature, the Macrogol 2000 through vacuum-drying cooling is added in flask, and add isophorone diisocyanate and catalyzer in flask, then be warming up to 60～80 ℃, reaction 1～4h, obtains base polyurethane prepolymer for use as;
Step 2: prepare alkane hydroxy silicon oil
In flask, add Di-n-Butyl Amine and epoxy double-seal head according to a certain percentage, be warming up to 60～100 ℃ of reaction 2～6h; Then to the octamethylcyclotetrasiloxane and the catalyzer that add certain mass in flask, be warming up to 110～130 ℃ of reaction 1～4h, obtain alkane hydroxy silicon oil;
Step 3: prepare urethane organosilicon multiple copolymer
The alkane hydroxy silicon oil that the base polyurethane prepolymer for use as that described step 1 is obtained and described step 2 obtain adds in flask according to a certain percentage, is then warming up to 50～80 ℃ of reaction 1～4h, obtains urethane organosilicon multiple copolymer;
Step 4: prepare polyurethane-modified organosilicon multiple copolymer fabric softener
In the organosilicon multiple copolymer obtaining to described step 3, add deionized water to be diluted to the solid content of needs, stirring and emulsifying, obtains.
2. the preparation method of a kind of polyurethane-modified organosilicon multiple copolymer fabric softener as claimed in claim 1, it is characterized in that, in described step 1, vacuum drying temperature is 110～120 ℃, vacuum tightness 0.08～0.09MPa, time is 2～4h, is cooled to 45～50 ℃ after vacuum-drying.
3. the preparation method of a kind of polyurethane-modified organosilicon multiple copolymer fabric softener as claimed in claim 1, is characterized in that, in described step 1, the mol ratio of isophorone diisocyanate and described Macrogol 2000 is 1.2～1.8:1.
4. the preparation method of a kind of polyurethane-modified organosilicon multiple copolymer fabric softener as claimed in claim 1, it is characterized in that, in described step 1, catalyzer is dibutyl tin dilaurate, and consumption is 1/2000～1/1000 of Macrogol 2000 and isophorone diisocyanate quality summation.
5. the preparation method of a kind of polyurethane-modified organosilicon multiple copolymer fabric softener as claimed in claim 1, is characterized in that, in described step 2, the mol ratio of Di-n-Butyl Amine and epoxy double-seal head is 1:1.
6. the preparation method of a kind of polyurethane-modified organosilicon multiple copolymer fabric softener as claimed in claim 1, is characterized in that, in described step 2, the mass ratio of octamethylcyclotetrasiloxane and epoxy double-seal head is 5～20:1.
7. the preparation method of a kind of polyurethane-modified organosilicon multiple copolymer fabric softener as claimed in claim 1, it is characterized in that, in described step 2, catalyzer is Tetramethylammonium hydroxide, and the quality of described catalyzer is with respect to 1/1000 of octamethylcyclotetrasiloxane quality.
8. the preparation method of a kind of polyurethane-modified organosilicon multiple copolymer fabric softener as claimed in claim 1, is characterized in that, in described step 3, the mol ratio of base polyurethane prepolymer for use as and alkane hydroxy silicon oil is 1:1.
9. the preparation method of a kind of polyurethane-modified organosilicon multiple copolymer fabric softener as claimed in claim 1, it is characterized in that, in described step 3, add catalyzer dibutyl tin dilaurate, the quality of described dibutyl tin dilaurate is 1/2000～1/1000 of base polyurethane prepolymer for use as and alkane hydroxy silicon oil quality summation.
10. the preparation method of a kind of polyurethane-modified organosilicon multiple copolymer fabric softener as claimed in claim 1, is characterized in that, in described step 4, churning time is 2～4h.
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Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104327238A (en) * | 2014-10-22 | 2015-02-04 | 齐鲁工业大学 | Preparation method for organosilicone positive ion waterborne polyurethane |
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| CN104327238A (en) * | 2014-10-22 | 2015-02-04 | 齐鲁工业大学 | Preparation method for organosilicone positive ion waterborne polyurethane |
| CN104327238B (en) * | 2014-10-22 | 2016-07-06 | 齐鲁工业大学 | A kind of preparation method of organosilicon cationic aqueous polyurethane |
| CN104341575A (en) * | 2014-10-23 | 2015-02-11 | 西安工程大学 | Synthesis method of water-based organosilicone polyurethane finishing agent for easily caring wool |
| CN104341575B (en) * | 2014-10-23 | 2017-02-15 | 江苏华鹿纺织有限公司 | Synthesis method of water-based organosilicone polyurethane finishing agent for easily caring wool |
| CN105693980A (en) * | 2016-04-14 | 2016-06-22 | 南通斯恩特纺织科技有限公司 | Blocked organosilicone waterborne polyurethane anti-fluffing-and-pilling agent |
| CN105693989A (en) * | 2016-04-14 | 2016-06-22 | 南通曙光染织有限公司 | Preparation method of blocked organosilicone waterborne polyurethane anti-fluffing-and-pilling agent |
| CN106432670A (en) * | 2016-09-16 | 2017-02-22 | 淄博鲁瑞精细化工有限公司 | Preparation method of organic silicon-modified polyurethane copolymer fabric softener |
| CN106521968A (en) * | 2016-12-14 | 2017-03-22 | 苏州陈恒织造有限公司 | Fabric softening agent and preparation method thereof |
| CN106948178A (en) * | 2017-04-25 | 2017-07-14 | 苏州依司特新材料科技有限公司 | Organic silicon modified polyurethane anti-pilling finishing agent, preparation method and application |
| CN107556483A (en) * | 2017-10-25 | 2018-01-09 | 威海诺葳信和新材料有限公司 | A kind of linear both sexes end carboxyl polyethers amido silicon oil, its crosslinking both sexes carboxyl polyethers amino silicone breast softening agent prepared and preparation method |
| CN107974837A (en) * | 2017-12-06 | 2018-05-01 | 佛山市顺德区德美瓦克有机硅有限公司 | One kind is containing polyurethane-modified Organosiliconcopolymere of quaternary ammonium salt and preparation method thereof |
| CN107974837B (en) * | 2017-12-06 | 2020-04-24 | 佛山市顺德区德美瓦克有机硅有限公司 | Polyurethane modified organic silicon copolymer containing quaternary ammonium salt and preparation method thereof |
| CN108659225A (en) * | 2018-05-25 | 2018-10-16 | 广州盛泰诺新材料科技有限公司 | A kind of electrostatic-resistant heat conducting silicone oil and its synthetic method |
| CN108951279A (en) * | 2018-07-11 | 2018-12-07 | 翟琳 | A kind of preparation method of papermaking softening agent |
| CN109736091A (en) * | 2019-01-22 | 2019-05-10 | 乐清市雅格狮丹服饰有限公司 | A kind of anti pilling overcoat and its treatment process |
| CN109797567A (en) * | 2019-01-24 | 2019-05-24 | 丹东优耐特纺织品有限公司 | A kind of high Waterproof Breathable, fire-retardant tent material processing and treating method |
| CN110128620A (en) * | 2019-05-17 | 2019-08-16 | 浙江理工大学 | A kind of preparation method of novel and multifunctional face-cloth softening agent for paper |
| CN110357919A (en) * | 2019-07-04 | 2019-10-22 | 大连振邦氟涂料股份有限公司 | A kind of preparation of siliceous ultraviolet absorber and its polyurethane copolymer |
| CN110591040A (en) * | 2019-09-29 | 2019-12-20 | 浙江理工大学 | Preparation method of environment-friendly type softening agent for antibacterial facial tissue |
| CN110904723A (en) * | 2019-10-28 | 2020-03-24 | 浙江理工大学 | Preparation method of super-moisturizing and high-antibacterial softening agent for facial tissues |
| CN112679696A (en) * | 2020-04-03 | 2021-04-20 | 胡黎明 | Preparation method of high-stability organosilicon modified waterborne polyurethane |
| CN111234167A (en) * | 2020-04-03 | 2020-06-05 | 胡黎明 | Preparation method of high-stability organic silicon modified waterborne polyurethane |
| CN112679695A (en) * | 2020-04-03 | 2021-04-20 | 胡黎明 | Preparation method of high-stability organic silicon modified waterborne polyurethane |
| CN112687854A (en) * | 2020-12-17 | 2021-04-20 | 广东微电新能源有限公司 | Silicon monoxide composite negative electrode material of lithium ion battery and preparation method and application thereof |
| CN115369664A (en) * | 2022-07-21 | 2022-11-22 | 海盐嘉源色彩科技股份有限公司 | Modal polyester knitted fabric peach skin tie-dyeing short-process technology |
| CN115369664B (en) * | 2022-07-21 | 2024-01-30 | 海盐嘉源色彩科技股份有限公司 | Short-process pad dyeing process for modal polyester knitted fabric peach skin |
| CN115612055A (en) * | 2022-10-11 | 2023-01-17 | 江苏富淼科技股份有限公司 | Solvent-free self-emulsified water-washing-resistant softening agent, and preparation method and application thereof |
| CN115819717A (en) * | 2022-10-11 | 2023-03-21 | 江苏富淼科技股份有限公司 | Washable daily softener, and preparation method and application thereof |
| CN115787301A (en) * | 2022-11-18 | 2023-03-14 | 杭州传化精细化工有限公司 | Polyurethane modified organic silicon softener and preparation method and application thereof |
| CN117188187A (en) * | 2023-09-08 | 2023-12-08 | 广东彩格科技有限公司 | Polyurethane composite printing paint and production process thereof |
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