CN109137530A - A kind of blocked isocyanate self-cross linking type one-way wet-guide agent and preparation method thereof - Google Patents

A kind of blocked isocyanate self-cross linking type one-way wet-guide agent and preparation method thereof Download PDF

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Publication number
CN109137530A
CN109137530A CN201810790044.7A CN201810790044A CN109137530A CN 109137530 A CN109137530 A CN 109137530A CN 201810790044 A CN201810790044 A CN 201810790044A CN 109137530 A CN109137530 A CN 109137530A
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China
Prior art keywords
parts
way wet
blocked isocyanate
cross linking
guide agent
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CN201810790044.7A
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CN109137530B (en
Inventor
何齐海
陈焜
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Hangzhou Meigao Huayi Chemical Co Ltd
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Hangzhou Meigao Huayi Chemical Co Ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/643Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
    • D06M15/653Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain modified by isocyanate compounds
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34Polyamides
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/50Modified hand or grip properties; Softening compositions

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Polyurethanes Or Polyureas (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The present invention relates to a kind of textile auxiliary fields, more particularly, to a kind of blocked isocyanate self-cross linking type one-way wet-guide agent and preparation method thereof.It is matched by weight: 100 parts of octamethylcy-clotetrasiloxane, 2~4 parts of 3- isocyanate group propyl-triethoxysilicane, 1,3- bis- (3- glycidylpropyl) -1,1,4~6 parts of 3,3- tetramethyl disiloxane, 10~15 parts of chain alkyl dimethyl silicone polymer, 0.5~1 part of potassium hydroxide, 0.6~2 part of methyl ethyl ketoxime, 1.5~3 parts of diethylenetriamine.Its product environmental performance is higher, further protects environment.

Description

A kind of blocked isocyanate self-cross linking type one-way wet-guide agent and preparation method thereof
Technical field
The present invention relates to a kind of textile auxiliary fields, more particularly, to a kind of blocked isocyanate self-cross linking type one-way wet-guide Agent and preparation method thereof.
Background technique
The wet guilding of fabric is an important indicator for measuring clothes level of comfort.Fabric energy with good wet transmitting performance The sweat that human body generates uniaxially is transmitted to the outer surface of fabric from the inner surface of fabric and is quickly spread, to keep human body skin Skin is dry, adjusts the comfort in human body micro climate area.Recent domestic researcher be all mostly by change fibre structure and Fabric structure realizes the one-way wet-guide of fabric.Although this fabric structure can be realized quick moisture absorption, unfavorable In the rapid evaporation of moisture.Currently, being arranged using one-way wet-guide finishing agent to fabric, by the parent for changing fabric ectonexine Hydrophobicity realizes the rapid evaporation of moisture.Common one-way wet-guide agent is fluorine-containing water repellent finishing agent, the finishing agent hydrophobicity Can be excellent, but easily accumulated in nature and organism, harm finally is generated to the mankind, does not meet the requirement of environmental regulation.
Summary of the invention
Object of the present invention is to customer service the deficiencies in the prior art, provide a kind of wash fast sealing end for meeting environmental regulation requirement Isocyanates self-cross linking type one-way wet-guide agent.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of blocked isocyanate self-cross linking type one-way wet-guide agent, is matched by weight:
100 parts of octamethylcy-clotetrasiloxane, 2~4 parts of 3- isocyanate group propyl-triethoxysilicane, (the 3- contracting of 1,3- bis- Water glycerol propyl) 4~6 parts of -1,1,3,3- tetramethyl disiloxane, 10~15 parts of chain alkyl dimethyl silicone polymer, hydrogen-oxygen Change 0.5~1 part of potassium, 0.6~2 part of methyl ethyl ketoxime, 1.5~3 parts of diethylenetriamine.
A kind of preparation method of blocked isocyanate self-cross linking type one-way wet-guide agent, including following synthetic method and step:
By octamethylcy-clotetrasiloxane, 3- isocyanate group propyl-triethoxysilicane, (the 3- glycidol third of 1,3- bis- Base) -1,1,3,3- tetramethyl disiloxane, chain alkyl dimethyl silicone polymer and potassium hydroxide are added in reaction vessel, 100~120 DEG C are heated to, after keeping the temperature 3~4h, then is cooled to 70~80 DEG C, methyl ethyl ketoxime is added dropwise, is added dropwise to complete rear insulation reaction 0.5~1h adds diethylenetriamine, and cooling discharge after 0.5~1h is kept the temperature at 70~80 DEG C, obtains blocked isocyanate certainly Cross-linking type one-way wet-guide agent.
Preferably, the molecular weight of the chain alkyl dimethyl silicone polymer is one in 8000,10000,12000 Kind.
Preferably, the one-way wet-guide agent is applied to nylon fabric.
The present invention uses 3- isocyanate group propyl-triethoxysilicane for self-cross linking monomer, is sealed using methyl ethyl ketoxime End, when high-temperature process, unseal, and are formed and are crosslinked with active hydrogen reactions such as amino, hydroxyls in system, improve fabric after arrangement The washing fastness of one-way wet-guide performance and smooth performance;The introducing of long chain alkane PolydimethylsiloxaneChain Chain section, provides for system Good hydrophobicity, and assign fabric preferable soft and smooth performance;It uses diethylenetriamine for chain extender, increases finishing agent While to the adsorptivity of fiber, and the isocyanate group that can be honored as a queen with solution reacts, and achievees the purpose that self-crosslinking.It reacted It not being needed in journey using solvent, no fluorochemical monomer participates in, the discharge of volatile organic compounds (VOC) in use process is reduced, Avoid the generation of perfluorooctanoic acid salt (PFOA), perfluorooctane sulfonyl compound (PFOS), safety and environmental protection.
Detailed description of the invention
Fig. 1 is the infrared spectrum of embodiment 1 in the present invention;
Fig. 2 is the infrared spectrum of embodiment 2 in the present invention;
Fig. 3 is the infrared spectrum of embodiment 3 in the present invention.
Specific embodiment
Below by specific embodiment, in conjunction with attached drawing, the present invention will be further described.
Embodiment 1:
By 100 parts of octamethylcy-clotetrasiloxanes, 2 parts of 3- isocyanate group propyl-triethoxysilicanes, 6 parts of bis- (3- of 1,3- Glycidylpropyl) -1,1,3,3- tetramethyl disiloxane, 12 parts of chain alkyl dimethyl silicone polymers and 0.8 part of hydroxide Potassium is added in reaction vessel, is heated to 120 DEG C, after keeping the temperature 3h, is cooled to 80 DEG C, 1 part of methyl ethyl ketoxime is added dropwise, after being added dropwise to complete Insulation reaction 0.5h adds 3 parts of diethylenetriamines, and cooling discharge after 1h is kept the temperature at 70 DEG C, obtains blocked isocyanate certainly Cross-linking type one-way wet-guide agent.
Referring to attached drawing 1, it is the infrared spectrogram of the present embodiment.As seen from the figure in 1259.16cm-1、1013.05cm-1、 797.35cm-1Place is three characteristic absorption peaks of organosilicon, 3384.25cm-1Place is the characteristic absorption peak of amino, 1698.94cm-1And 1530cm-1Place is the characteristic absorption peak of carbamate groups, 697.38cm-1It is nearby the characteristic absorption peak of long chain alkane. The bright target product of summary analysis successfully obtains.
Embodiment 2:
By 100 parts of octamethylcy-clotetrasiloxanes, 4 parts of 3- isocyanate group propyl-triethoxysilicanes, 4 parts of bis- (3- of 1,3- Glycidylpropyl) -1,1,3,3- tetramethyl disiloxane, 15 parts of chain alkyl dimethyl silicone polymers and 1 part of potassium hydroxide It is added in reaction vessel, is heated to 120 DEG C, after keeping the temperature 3h, be cooled to 80 DEG C, 2 parts of methyl ethyl ketoximes are added dropwise, are protected after being added dropwise to complete Temperature reaction 1h, adds 2 parts of diethylenetriamines, and cooling discharge after 1h is kept the temperature at 70 DEG C, obtains blocked isocyanate self-crosslinking Type one-way wet-guide agent;
Referring to attached drawing 2, it is the infrared spectrogram of the present embodiment.As seen from the figure in 1259.24cm-1、1016.60cm-1、 785.95cm-1Place is three characteristic absorption peaks of organosilicon, 3374.31cm-1Place is the characteristic absorption peak of amino, 1696.54cm-1And 1535.07cm-1Place is the characteristic absorption peak of carbamate groups, 699.91cm-1It is nearby the characteristic absorption of long chain alkane Peak.The bright target product of summary analysis successfully obtains.
Embodiment 3:
By 100 parts of octamethylcy-clotetrasiloxanes, 3 parts of 3- isocyanate group propyl-triethoxysilicanes, 5 parts of bis- (3- of 1,3- Glycidylpropyl) -1,1,3,3- tetramethyl disiloxane, 15 parts of chain alkyl dimethyl silicone polymers and 1 part of potassium hydroxide It is added in reaction vessel, is heated to 110 DEG C, after keeping the temperature 4h, be cooled to 80 DEG C, 1.5 parts of methyl ethyl ketoximes be added dropwise, after being added dropwise to complete Insulation reaction 1h adds 2 parts of diethylenetriamines, and cooling discharge after 1h is kept the temperature at 80 DEG C, obtains blocked isocyanate selfing Connection type one-way wet-guide agent;
Referring to attached drawing 3, it is the infrared spectrogram of the present embodiment.As seen from the figure in 1259.25cm-1、1016.60cm-1、 800.78cm-1Place is three characteristic absorption peaks of organosilicon, 3374.16cm-1Place is the characteristic absorption peak of amino, 1696.40cm-1And 1535.00cm-1Place is the characteristic absorption peak of carbamate groups, 699.74cm-1It is nearby the characteristic absorption of long chain alkane Peak.The bright target product of summary analysis successfully obtains.Finisher is applied in a kind of blocked isocyanate self-cross linking type one-way wet-guide agent Skill:
1. leading the preparation of humectant lotion
2. finishing technique
Fabric used: nylon woven fabric.
Finishing technique process: reverse side water repellent finish → bake (170 DEG C × 60s) → washing drying
→ front hydrophilic finiss → bakes (170 DEG C × 60s) → test
Reverse side water repellent finish prescription (g/L):
Lead humectant lotion 50
Thickener 15
Front hydrophilic finiss prescription (g/L)
Moisture control agent M-5900 20
3. application performance test
Penetrability uses LLY211 type moisture vapor transmission cup, according to GB/T 12704-1991 " fabric moisture transmission quantity measuring method moisture vapor transmission cup Method A moisture absorption method " it is tested.
Diffusion time and dilation angle drip with reference to the GB/T 21655.1-2008 " evaluation the 1st of textile absorbing fast-drying Part: individual event composite test method ".
Flexible appraisal: it is evaluated with hand digital palpation for examination of trauma, using 1~5 point of judge method, 1 point worst, and 5 points best, the same news commentary of three people It is fixed, it makes even respectively.
Washing fastness: it is tested with reference to GB/T3921.1-1997 " textile color stability test color fastness to washing ".
The results are shown in Table 1 for blocked isocyanate self-cross linking type one-way wet-guide agent application performance test of the invention:
1 blocked isocyanate self-cross linking type one-way wet-guide agent application performance test result of table
As can be seen from the above table, the fabric after blocked isocyanate self-cross linking type one-way wet-guide agent of the present invention arrangement, tool There is good water droplet wetability, show the good hydrophilic property of fabric, analyzes in conjunction with vapor transfer rate it is found that its one-way wet-guide better performances. Fabric feeling is obviously improved after arranging simultaneously, and it is small to decline degree after washing.

Claims (4)

1. a kind of blocked isocyanate self-cross linking type one-way wet-guide agent, which is characterized in that matched by weight:
(3- shrinks sweet by 100 parts of octamethylcy-clotetrasiloxane, 2~4 parts of 3- isocyanate group propyl-triethoxysilicane, 1,3- bis- Oily propyl) 4~6 parts of -1,1,3,3- tetramethyl disiloxane, 10~15 parts of chain alkyl dimethyl silicone polymer, potassium hydroxide 0.5~1 part, 0.6~2 part of methyl ethyl ketoxime, 1.5~3 parts of diethylenetriamine.
2. a kind of preparation method of blocked isocyanate self-cross linking type one-way wet-guide agent according to claim 1, feature It is, including following synthetic method and step:
By octamethylcy-clotetrasiloxane, 3- isocyanate group propyl-triethoxysilicane, 1,3- bis- (3- glycidylpropyl) -1, 1,3,3- tetramethyl disiloxane, chain alkyl dimethyl silicone polymer and potassium hydroxide are added in reaction vessel, are heated to 100~120 DEG C, after keeping the temperature 3~4h, then be cooled to 70~80 DEG C, methyl ethyl ketoxime be added dropwise, be added dropwise to complete rear insulation reaction 0.5~ 1h adds diethylenetriamine, and cooling discharge after 0.5~1h is kept the temperature at 70~80 DEG C, obtains blocked isocyanate self-crosslinking Type one-way wet-guide agent.
3. a kind of preparation method of blocked isocyanate self-cross linking type one-way wet-guide agent according to claim 1, feature Be: the molecular weight of the chain alkyl dimethyl silicone polymer is one of 8000,10000,12000.
4. a kind of preparation method of blocked isocyanate self-cross linking type one-way wet-guide agent according to claim 1, feature Be: the one-way wet-guide agent is applied to nylon fabric.
CN201810790044.7A 2018-07-18 2018-07-18 Blocked isocyanate self-crosslinking unidirectional moisture-transfer agent and preparation method thereof Active CN109137530B (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61282480A (en) * 1985-06-06 1986-12-12 株式会社 バイロン Water-proof and antistatic coating composition of fiber product and processing of fiber product by said composition
US4985155A (en) * 1988-03-17 1991-01-15 Nissin Chemical Industry Co., Ltd. Silicone-containing fabric finishing agent
CN1396958A (en) * 2000-01-27 2003-02-12 拜尔公司 Polysiloxanes used for hydrophobing
CN103351461A (en) * 2013-06-26 2013-10-16 佛山市顺德区德美瓦克有机硅有限公司 Blocked isocyanate modified polyether organic silicon and preparation method thereof
CN104650364A (en) * 2015-02-05 2015-05-27 南通斯恩特纺织科技有限公司 Preparation method of hyper-branched polyether amide block silicone
CN105037679A (en) * 2015-09-23 2015-11-11 苏州依司特新材料科技有限公司 Cationic type polyurethane modified organosilicon water repellent agent and preparation method and application thereof
CN105504291A (en) * 2016-01-19 2016-04-20 淮安凯悦科技开发有限公司 Linear block amino silicone oil softening agent as well as preparation method and application thereof
CN106049069A (en) * 2016-07-15 2016-10-26 北京理工大学 Fluorine-free fabric water repellent with branched structure and preparation method of fluorine-free fabric water repellent

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61282480A (en) * 1985-06-06 1986-12-12 株式会社 バイロン Water-proof and antistatic coating composition of fiber product and processing of fiber product by said composition
US4985155A (en) * 1988-03-17 1991-01-15 Nissin Chemical Industry Co., Ltd. Silicone-containing fabric finishing agent
CN1396958A (en) * 2000-01-27 2003-02-12 拜尔公司 Polysiloxanes used for hydrophobing
CN103351461A (en) * 2013-06-26 2013-10-16 佛山市顺德区德美瓦克有机硅有限公司 Blocked isocyanate modified polyether organic silicon and preparation method thereof
CN104650364A (en) * 2015-02-05 2015-05-27 南通斯恩特纺织科技有限公司 Preparation method of hyper-branched polyether amide block silicone
CN105037679A (en) * 2015-09-23 2015-11-11 苏州依司特新材料科技有限公司 Cationic type polyurethane modified organosilicon water repellent agent and preparation method and application thereof
CN105504291A (en) * 2016-01-19 2016-04-20 淮安凯悦科技开发有限公司 Linear block amino silicone oil softening agent as well as preparation method and application thereof
CN106049069A (en) * 2016-07-15 2016-10-26 北京理工大学 Fluorine-free fabric water repellent with branched structure and preparation method of fluorine-free fabric water repellent

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