CN109320725A - A kind of safe mixed solvent is used for block silicone oil synthesis technology - Google Patents
A kind of safe mixed solvent is used for block silicone oil synthesis technology Download PDFInfo
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- CN109320725A CN109320725A CN201811260751.1A CN201811260751A CN109320725A CN 109320725 A CN109320725 A CN 109320725A CN 201811260751 A CN201811260751 A CN 201811260751A CN 109320725 A CN109320725 A CN 109320725A
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- silicone oil
- mixed solvent
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- block silicone
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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
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/46—Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
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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
- D06M15/647—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing polyether sequences
-
- 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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- 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)
- Silicon Polymers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention provides a kind of safe mixed solvent for block silicone oil synthesis technology; the following steps are included: step (1): according to quality proportioning: in the case where 45-50 parts of isopropanols are solvent condition; by 31-37 parts of Amino End Group silicone oil, 65-83 parts of end epoxidized polyethers, 65-83 parts of end epoxyalkane, put into equipped with blender, thermometer, condenser pipe four-hole boiling flask in; under nitrogen protection; stirring is warming up to 80 DEG C or so; insulation reaction 15-16 hours; after heat preservation; cooling, obtains the ternary polymerization silicon oil solution of low concentration；Step (2): the ternary polymerization silicon oil solution of low concentration is evaporated under reduced pressure, after removing partial solvent according to required concentration, the mixed solvent of 25-42 parts of safety is added immediately, after mixing evenly, up to transparent, faint yellow sticky linear multiple block copolymerization organosilicon, after fabric uses tri-block silicone oil prepared by the present invention, have the characteristics that good hand touch, good hydrophilic property, low-yellowing, and the mixed solvent of safety can assign fabric certain ice sense.
Description
Technical field
The present invention relates to fabric care agent technical field, specially a kind of safe mixed solvent is synthesized for block silicone oil
Technique.
Background technique
For chemical fibre hydrophilic softening agent for a long time always based on the aqueous solution of polyester polyether block polymer, the type is soft
The structure of agent is mainly made of two parts: polyester construction is used for the anchorage effect to chemical fiber, macromolecular polyethers as anchorage
Group provides hydrophilic radical, while providing some flexibility feels.But with increasingly requiring multiple demands, the product
Disadvantage is also increasingly prominent, only soft feel, and smooth performance can not provide.Based on the demand of richer feel feature, exploitation one
Branch chemical fibre hydrophilic silicon oil is at the task of top priority.
Hydrophilic class softening agent is generally pendant polyether modified silicon oil (market is commonly called as CGF) and pendant polyether modified amido silicon
Based on oils, this kind of softening agent hydrophily is preferable, but arrange after fabric feel it is undesirable, which greatly limits it
Further apply.
Summary of the invention
Technical problem solved by the invention is to provide a kind of safe mixed solvent for block silicone oil synthesis technology,
To solve the problems in above-mentioned background technique.
Technical problem solved by the invention is realized using following technical scheme: a kind of safe mixed solvent is for embedding
Section silicone oil synthesis technology, comprising the following steps:
Step (1): according to quality proportioning: in the case where 45-50 parts of isopropanols are solvent condition, by 31-37 parts of Amino End Group silicone oil, 65-
83 parts of end epoxidized polyethers, 65-83 parts of end epoxyalkane, put into equipped with blender, thermometer, condenser pipe four-hole boiling flask in,
Under nitrogen protection, stirring is warming up to 80 DEG C or so, and insulation reaction 15-16 hours, after heat preservation, cooling obtained low concentration
Ternary polymerization silicon oil solution；
Step (2): the ternary polymerization silicon oil solution of low concentration is evaporated under reduced pressure, and removes partial solvent according to required concentration
Afterwards, the mixed solvent of 25-42 parts of safety is added immediately, after mixing evenly to get transparent, faint yellow sticky linear multiple block
It is copolymerized organosilicon, solid content is 55%~60%；Terpolymer block silicone oil molecular weight is 15000~25000g/mol.
Step (1) the middle-end amido silicon oil molecular weight is 1990-2500g/mol.
Step (1) the middle-end epoxidized polyether 1200-1500g/mol.
Amino End Group silicone oil/end epoxidized polyether/end epoxyalkane molar ratio in the step (1) is 1:2:2~1:
2.2:2.2。
Safe mixed solvent in the step (2) is isopropanol, hexylene glycol, and mass ratio is isopropanol: dissident
Glycol=1:1-1:5.
Be compared to open technology, there are following advantages by the present invention: fabric uses tri-block silicone oil prepared by the present invention
Afterwards, have the characteristics that good hand touch, good hydrophilic property, low-yellowing, and the mixed solvent of safety can assign fabric certain ice sense.
Specific embodiment
In order to make, technological means of the invention, creation characteristic, workflow, application method reach purpose and effect is easy to bright
White understanding, below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " company ", " connection "
It shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected to be mechanical connection,
It is also possible to be electrically connected;It can be directly connected, can also indirectly connected through an intermediary, it can company inside two elements
It is logical, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention
In embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
Embodiment 1
A kind of safe mixed solvent is used for block silicone oil synthesis technology, comprising the following steps:
Step (1): according to quality proportioning: in the case where 45-50 parts of isopropanols are solvent condition, by 31-37 parts of Amino End Group silicone oil, 65-
83 parts of end epoxidized polyethers, 65-83 parts of end epoxyalkane, put into equipped with blender, thermometer, condenser pipe four-hole boiling flask in,
Under nitrogen protection, stirring is warming up to 80 DEG C or so, and insulation reaction 15-16 hours, after heat preservation, cooling obtained low concentration
Ternary polymerization silicon oil solution；Amino End Group silicone molecule amount is 1990-2500g/mol；Hold epoxidized polyether 1200-1500g/mol；
Amino End Group silicone oil/end epoxidized polyether/end epoxyalkane molar ratio is 1:2:2.
Step (2): the ternary polymerization silicon oil solution of low concentration is evaporated under reduced pressure, molten according to required concentration removing part
After agent, the mixed solvent of 25-42 parts of safety is added immediately, it is embedding to get transparent, faint yellow sticky linear multiple after mixing evenly
Duan Gongju organosilicon, solid content is 55%~60%；Terpolymer block silicone oil molecular weight is 15000~25000g/mol；Peace
Full mixed solvent is isopropanol, hexylene glycol, and mass ratio is isopropanol: hexylene glycol=1:5.
Embodiment 2
A kind of safe mixed solvent is used for block silicone oil synthesis technology, comprising the following steps:
Step (1): according to quality proportioning: in the case where 45-50 parts of isopropanols are solvent condition, by 31-37 parts of Amino End Group silicone oil, 65-
83 parts of end epoxidized polyethers, 65-83 parts of end epoxyalkane, put into equipped with blender, thermometer, condenser pipe four-hole boiling flask in,
Under nitrogen protection, stirring is warming up to 80 DEG C or so, and insulation reaction 15-16 hours, after heat preservation, cooling obtained low concentration
Ternary polymerization silicon oil solution；Amino End Group silicone molecule amount is 1990-2500g/mol；Hold epoxidized polyether 1200-1500g/mol；
Amino End Group silicone oil/end epoxidized polyether/end epoxyalkane molar ratio is 1:2:2.
Step (2): the ternary polymerization silicon oil solution of low concentration is evaporated under reduced pressure, molten according to required concentration removing part
After agent, the mixed solvent of 25-42 parts of safety is added immediately, it is embedding to get transparent, faint yellow sticky linear multiple after mixing evenly
Duan Gongju organosilicon, solid content is 55%~60%；Terpolymer block silicone oil molecular weight is 15000~25000g/mol；Peace
Full mixed solvent is isopropanol, hexylene glycol, and mass ratio is isopropanol: hexylene glycol=1:1.
Embodiment 3
A kind of safe mixed solvent is used for block silicone oil synthesis technology, comprising the following steps:
Step (1): according to quality proportioning: in the case where 45-50 parts of isopropanols are solvent condition, by 31-37 parts of Amino End Group silicone oil, 65-
83 parts of end epoxidized polyethers, 65-83 parts of end epoxyalkane, put into equipped with blender, thermometer, condenser pipe four-hole boiling flask in,
Under nitrogen protection, stirring is warming up to 80 DEG C or so, and insulation reaction 15-16 hours, after heat preservation, cooling obtained low concentration
Ternary polymerization silicon oil solution；Amino End Group silicone molecule amount is 1990-2500g/mol；Hold epoxidized polyether 1200-1500g/mol；
Amino End Group silicone oil/end epoxidized polyether/end epoxyalkane molar ratio is 1:2.2:2.2.
Step (2): the ternary polymerization silicon oil solution of low concentration is evaporated under reduced pressure, molten according to required concentration removing part
After agent, the mixed solvent of 25-42 parts of safety is added immediately, it is embedding to get transparent, faint yellow sticky linear multiple after mixing evenly
Duan Gongju organosilicon, solid content is 55%~60%；Terpolymer block silicone oil molecular weight is 15000~25000g/mol；Peace
Full mixed solvent is isopropanol, hexylene glycol, and mass ratio is isopropanol: hexylene glycol=1:5.
Fabric after collated dose is arranged is laid in desktop, with standard dropper (25 drops/ml) from from fabric 3cm height
It drips to fabric surface drop 1, measurement fabric has absorbed 1 and dripped the time used under quiescent conditions.By chemical fibre hydrophilic silicone oil
Fabric after arrangement also has good hydrophily, this is and contains a large amount of polyether groups and cation quaternary ammonium salt in its structure
Group be determine, the hydrophilicity having had, at the same with the binding ability of fiber also relatively by force, so its wash durability compared with
It is good；Fabric hydrophilic after the arrangement of pendant polyether amido silicon oil is poorer than polyether silicone oil, this is because in its molecular structure not only
With a large amount of secondary amine salt groups, also there is polyether group, hydrophilicity is good, while also having certain washing fastness.
The above shows and describes the basic principle, main features and advantages of the invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.Claimed range of the invention by appended claims and
Its equivalent thereof.
Claims (5)
1. a kind of safe mixed solvent is used for block silicone oil synthesis technology, it is characterised in that: the following steps are included:
Step (1): according to quality proportioning: in the case where 45-50 parts of isopropanols are solvent condition, by 31-37 parts of Amino End Group silicone oil, 65-
83 parts of end epoxidized polyethers, 65-83 parts of end epoxyalkane, put into equipped with blender, thermometer, condenser pipe four-hole boiling flask in,
Under nitrogen protection, stirring is warming up to 80 DEG C or so, and insulation reaction 15-16 hours, after heat preservation, cooling obtained low concentration
Ternary polymerization silicon oil solution；
Step (2): the ternary polymerization silicon oil solution of low concentration is evaporated under reduced pressure, and removes partial solvent according to required concentration
Afterwards, the mixed solvent of 25-42 parts of safety is added immediately, after mixing evenly to get transparent, faint yellow sticky linear multiple block
It is copolymerized organosilicon, solid content is 55%~60%；Terpolymer block silicone oil molecular weight is 15000~25000g/mol.
2. a kind of safe mixed solvent according to claim 1 is used for block silicone oil synthesis technology, it is characterised in that: institute
Stating step (1) middle-end amido silicon oil molecular weight is 1990-2500g/mol.
3. a kind of safe mixed solvent according to claim 1 is used for block silicone oil synthesis technology, it is characterised in that: institute
State step (1) middle-end epoxidized polyether 1200-1500g/mol.
4. a kind of safe mixed solvent according to claim 1 is used for block silicone oil synthesis technology, it is characterised in that: institute
Stating Amino End Group silicone oil/end epoxidized polyether/end epoxyalkane molar ratio in step (1) is 1:2:2~1:2.2:2.2.
5. a kind of safe mixed solvent according to claim 1 is used for block silicone oil synthesis technology, it is characterised in that: institute
Stating the safe mixed solvent in step (2) is isopropanol, hexylene glycol, and mass ratio is isopropanol: hexylene glycol=1:1-1:
5。
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| CN201811260751.1A CN109320725A (en) | 2018-10-26 | 2018-10-26 | A kind of safe mixed solvent is used for block silicone oil synthesis technology |
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| CN201811260751.1A CN109320725A (en) | 2018-10-26 | 2018-10-26 | A kind of safe mixed solvent is used for block silicone oil synthesis technology |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114232139A (en) * | 2021-12-16 | 2022-03-25 | 连云港神鹰复合材料科技有限公司 | Preparation method of carbon fiber oil for dry-jet wet-spun precursor |
| CN114990889A (en) * | 2022-06-21 | 2022-09-02 | 广东创新精细化工实业有限公司 | Adhesive hydrophilic softening agent, preparation method thereof and application of adhesive hydrophilic softening agent in nylon fabric |
| CN116003804A (en) * | 2022-12-31 | 2023-04-25 | 浙江汉邦新材料股份有限公司 | Hydrophilic dustproof silicone oil finishing agent for fabric and preparation method thereof |
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| US20110265273A1 (en) * | 2008-11-21 | 2011-11-03 | Duplus Chemical Co., Ltd. Of Zhangjiagang City | Modifier for polyester fiber as well as preparation method and application of the same |
| CN106146856A (en) * | 2016-08-03 | 2016-11-23 | 清远市宏图助剂有限公司 | A kind of terpolymer block hydrophilic amino silicone oil and its preparation method and application |
| CN106750325A (en) * | 2016-12-12 | 2017-05-31 | 辽宁科隆精细化工股份有限公司 | A kind of method that use complex solvent prepares terpolymer block silicone oil |
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2018
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20110265273A1 (en) * | 2008-11-21 | 2011-11-03 | Duplus Chemical Co., Ltd. Of Zhangjiagang City | Modifier for polyester fiber as well as preparation method and application of the same |
| CN106146856A (en) * | 2016-08-03 | 2016-11-23 | 清远市宏图助剂有限公司 | A kind of terpolymer block hydrophilic amino silicone oil and its preparation method and application |
| CN106750325A (en) * | 2016-12-12 | 2017-05-31 | 辽宁科隆精细化工股份有限公司 | A kind of method that use complex solvent prepares terpolymer block silicone oil |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114232139A (en) * | 2021-12-16 | 2022-03-25 | 连云港神鹰复合材料科技有限公司 | Preparation method of carbon fiber oil for dry-jet wet-spun precursor |
| CN114990889A (en) * | 2022-06-21 | 2022-09-02 | 广东创新精细化工实业有限公司 | Adhesive hydrophilic softening agent, preparation method thereof and application of adhesive hydrophilic softening agent in nylon fabric |
| CN114990889B (en) * | 2022-06-21 | 2024-01-26 | 广东创新精细化工实业有限公司 | Rubberizing hydrophilic softener, preparation method thereof and application thereof in nylon fabric |
| CN116003804A (en) * | 2022-12-31 | 2023-04-25 | 浙江汉邦新材料股份有限公司 | Hydrophilic dustproof silicone oil finishing agent for fabric and preparation method thereof |
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Application publication date: 20190212 |
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