CN106750325A - A kind of method that use complex solvent prepares terpolymer block silicone oil - Google Patents
A kind of method that use complex solvent prepares terpolymer block silicone oil Download PDFInfo
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- CN106750325A CN106750325A CN201611136116.3A CN201611136116A CN106750325A CN 106750325 A CN106750325 A CN 106750325A CN 201611136116 A CN201611136116 A CN 201611136116A CN 106750325 A CN106750325 A CN 106750325A
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- silicone oil
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- complex solvent
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
- C08J3/095—Oxygen containing compounds
-
- 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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
-
- 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)
- General Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Silicon Polymers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention discloses a kind of method that use complex solvent prepares terpolymer block silicone oil; 1) step is under solvent condition; add double envelope epoxy-terminated silicone oil and polyetheramines; under nitrogen protection; in 80~85 DEG C, after 6~8h of reaction, 60~66 DEG C are cooled to; reduced vacuum treatment, removes partial solvent；Then step 2) add complex solvent to stir, terpolymer block silicone oil solution is finally given, 55%~60%, terpolymer block silicone oil molecular weight is about 12000~21000g/mol to solid content.After the tri-block silicone oil that fabric is prepared using the present invention, the features such as with good hand touch, good hydrophilic property, low-yellowing, and high boiling solvent in complex solvent can assign fabric certain ice sense.
Description
Technical field
The invention belongs to technical field of textile chemical engineering, and in particular to one kind prepares terpolymer block silicon using complex solvent
The method of oil.
Background technology
Silicone oil is widely used as a kind of softening agent in textile industry.Silicone oil can improve fabric feeling, and to human body
It is harmless.But general silicone oil has hydrophobicity, the water imbibition influence on fabric is larger, and easily xanthochromia.It is common by ternary
The modified silicone oil of poly block, there is a very big lifting in performance, but the terpolymer block silicone oil of some macromolecules from breast
The performances such as the property changed, hydrophily and stability need to improve.
The content of the invention
For drawbacks described above, by the present invention in that with complex solvent and the mode of increase polyetheramine molecular weight, being carried with reaching
The purpose of the hydrophily, self-emulsifying and stability of terpolymer block silicone oil high.
The technical solution adopted by the present invention is：
A kind of method that use complex solvent prepares terpolymer block silicone oil, comprises the following steps：
1) under conditions of solvent, epoxy radicals end-blocking silicone oil and polyetheramine are added, it is under nitrogen protection, anti-in 80~85 DEG C
6~8h is answered, the ternary polymerization silicon oil solution of low concentration is obtained；
2) the ternary polymerization silicon oil solution of low concentration is carried out into vacuum distillation, after removing partial solvent according to required concentration,
Complex solvent is added immediately, after stirring, obtains terpolymer block silicone oil solution.
Described method, step 1) in solvent for isopropanol or isopropanol it is molten with the mixing of of a relatively high boiling point solvent
Agent, the of a relatively high boiling point solvent is dipropylene glycol methyl ether and/or propylene glycol monomethyl ether.
Described method, step 1) the polyetheramine molecular weight be 2003g/mol.
Described method, step 1) epoxy-capped silicone oil molecular weight be 8000~17000g/mol.
Described method, step 1) in the mol ratio of epoxy-capped silicone oil and polyetheramine be 1:2~2.2.
Described method, step 2) in complex solvent be absolute ethyl alcohol, dipropylene glycol methyl ether and dipropylene.
Described method, the complex solvent is also wrapped in addition to absolute ethyl alcohol, dipropylene glycol methyl ether and dipropylene
Include one or more combinations in propylene glycol monomethyl ether, propandiol butyl ether, DPG.
Described method, the mass ratio of absolute ethyl alcohol, dipropylene glycol methyl ether and dipropylene is 6~8:2~3:1~
2。
Described method, the molecular weight for obtaining terpolymer block silicone oil solution is 12000~21000g/mol.
The invention has the advantages that；
The method that a kind of use complex solvent of the present invention prepares terpolymer block silicone oil, using under solvent condition, plus
Enter the silicone oil and polyetheramine of epoxy radicals end-blocking, according to mol ratio 1:2~2.2 add, under nitrogen protection, 80~85 DEG C of reactions 6
~8h, obtains the relatively low ternary polymerization silicone oil of concentration；Products therefrom is carried out into vacuum distillation, is removed according to required concentration a certain amount of
Solvent after, according still further to required complex solvent in every kind of solvent ratios enter line replacement solvent, obtain pale yellow transparent ternary be total to
Silicone oil.The solvent that it is used is isopropanol or isopropanol and a certain amount of dipropylene glycol methyl ether, propylene glycol monomethyl ether etc. boil
The mixture of the of a relatively high solvent of point.Epoxy-capped silicone molecule amount is 8000~17000g/mol, polyetheramine molecular weight
It is 2003g/mol.Complex solvent includes 6~8 parts of absolute ethyl alcohols, 2~3 parts of dipropylene glycol methyl ethers, 1~2 part of DPG fourth
Ether equal solvent, and in the ternary polymerization silicone oil for finally giving in addition to these solvents, also contain 10~15 parts or so of isopropanol.Most
The ternary polymerization silicone molecule amount for obtaining eventually is about 12000~21000g/mol.The modified silicon oil has the polyethers of certain length
Chain and silica chain so that the silicone oil has self-emulsifying, stability and hydrophily as finishing agent, while can also have a fabric
Certain ice sense.
Ternary polymerization silicone oil obtained by the present invention contains amino group because containing pfpe molecule chain more long, so tool
There is hydrophily；Due to using complex solvent, the ternary polymerization silicone oil can be with self-emulsifying, and emulsion is relatively stablized, while in complex solvent
High boiling solvent can also to a certain extent improve the ice sense of fabric.
Specific embodiment
A kind of method that use complex solvent prepares terpolymer block silicone oil, comprises the following steps that：
1) take 15~20 parts of epoxy radicals end-blocking silicone oil (8000~17000g/mol of molecular weight), ED2003 polyetheramines 4.5~
10 parts, 100~120 parts of isopropanol, under nitrogen protection, in 80~85 DEG C, react 6~8h, obtain the ternary polymerization of low concentration
Silicon oil solution；
2) 6~8 parts of absolute ethyl alcohols, 2~3 parts of dipropylene glycol methyl ethers, 1~2 part of dipropylene equal solvent mixing are taken to match somebody with somebody
It is made complex solvent；
3) the ternary polymerization silicon oil solution of the low concentration that will 1) obtain is cooled to 60~66 DEG C, reduced vacuum treatment, removing
90~100 parts of isopropanol；Complex solvent being added immediately, being stirred, (molecular weight is about to obtain terpolymer block silicone oil solution
It is 12000~21000g/mol).
Wherein, step 1) in ED2003 polyetheramines addition it is relevant with the molecular weight of epoxy radicals end-blocking silicone oil, epoxy radicals envelope
End silicone oil is 1 with the mol ratio of ED2003 polyetheramines:2~2.2.Step 2) used in complex solvent except add 6~8 parts of nothings
Outside water-ethanol, 2~3 parts of dipropylene glycol methyl ethers, 1~2 part of dipropylene, a small amount of propylene glycol monomethyl ether, propane diols are additionally added
Butyl ether, DPG etc..
With reference to example, implementation of the invention is described in detail.
The method that a kind of use complex solvent of embodiment 1 prepares terpolymer block silicone oil
Step is as follows：
1) epoxy-capped silicone oil (molecular weight 8000g/mol) 200g, ED2003 polyetheramine 100g and isopropanol 1200g is taken,
Under nitrogen protection, it is placed in the reactor with condensing unit, 85 DEG C of reaction 8h, the ternary polymerization silicone oil for obtaining low concentration is molten
Liquid；
2) 60g absolute ethyl alcohols, 30g dipropylene glycol methyl ethers, 10g dipropylenes are taken and is configured to complex solvent；
3) by step 1) the ternary polymerization silicon oil solution of low concentration for preparing is cooled to 60~66 DEG C, vacuum distillation, removing
1000g isopropanols, immediately add step 2) prepare complex solvent, stir, obtain ternary polymerization silicon oil solution.The ternary
Copolymerization silicone molecule amount is about 12142g/mol.
The method that a kind of use complex solvent of embodiment 2 prepares terpolymer block silicone oil
Step is as follows：
1) epoxy-capped silicone oil (molecular weight 10000g/mol) 200g, ED2003 polyetheramine 80.2g and isopropanol are taken
1200g, under nitrogen protection, is placed in the reactor with condensing unit, 85 DEG C of reaction 8h, obtains the ternary polymerization of low concentration
Silicon oil solution；
2) 80g absolute ethyl alcohols, 30g dipropylene glycol methyl ethers, 10g dipropylenes are taken and is configured to complex solvent；
3) by step 1) in the ternary polymerization silicon oil solution of low concentration be cooled to 60~66 DEG C, vacuum distillation removes 1000g
Isopropanol, immediately add step 2) prepare complex solvent, stir, obtain ternary polymerization silicon oil solution.The ternary polymerization
Silicone molecule amount is about 14346g/mol.
The method that a kind of use complex solvent of embodiment 3 prepares terpolymer block silicone oil
Step is as follows：
1) epoxy-capped silicone oil (molecular weight 10000g/mol) 200g, ED2003 polyetheramine 80.2g and isopropanol are taken
1200g, under nitrogen protection, is placed in the reactor with condensing unit, 85 DEG C of reaction 8h, obtains the ternary polymerization of low concentration
Silicon oil solution；
2) 80g absolute ethyl alcohols, 30g dipropylene glycol methyl ethers, 10g dipropylenes, 5g propylene glycol monomethyl ethers and 5g dipropyls are taken
Glycol is configured to complex solvent；
3) by step 1) the ternary polymerization silicon oil solution of low concentration for preparing is cooled to 60~66 DEG C, vacuum distillation, removing
950g isopropanols, immediately add step 2) prepare complex solvent, stir, obtain ternary polymerization silicon oil solution.The ternary
Copolymerization silicone molecule amount is about 14628g/mol.
Comparative example
It is 5% that the finishing agent ternary polymerization silicon oil solution that embodiment 1 to embodiment 3 is obtained is configured to mass fraction respectively
The aqueous solution, woven dacron and dacron thread are respectively placed in each aqueous finish solution and soak 20min, fabric is dried with rolling drying machine
Afterwards, in 2h is dried at 100 DEG C, shape 3s at 230 DEG C.Table one is through the woven dacron after the arrangement of each aqueous finish solution and washs
The correction data of synthetic fibre silk and the blank group performance without any finishing agent, table two is embodiment 1 molten using compounding to embodiment 3
The physicochemical property of the terpolymer block silicone oil aqueous solution prepared by liquid.
Method of testing is as follows：
Measuring brightness：With reference to the objective ranking method of the relative whiteness of GB/T8424.2-2001 textile color stabilities experiment.
Hydrophily is determined：With reference to AATCC79《The absorbability test of white goods》Determine, to absorb water, diffusion time represents.
Hand feel measurement：It is a small group with 3~5 people, closes mesh and touch the fabric after arranging, carries out hand feel evaluation.Hand feel evaluation
Carried out in terms of flexibility and smooth feeling two, be divided into 5 grades, series is bigger, represent that feel is better.
Dewatering ability is determined：The observation terpolymer block silicone oil aqueous solution is centrifuged under 3000r/min speed conditions
Stability after 45min.
Table one：
Table two：
From table one and two, collated dose arrange after fabric whiteness have slightly decline, low-yellowing, but feel has significantly
Lifting.The dewatering ability and self-emulsifying of aqueous finish solution are good, and its aqueous solution is transparent and with blue light.
Above content is better embodiment of the invention, for those skilled in the art, according to side of the invention
Method, various modifications are also had in specific embodiment and using upper, but this specification should not be construed as limitation of the invention, this
A little modifications are all contained within apllied interest field.
Claims (9)
1. a kind of method that use complex solvent prepares terpolymer block silicone oil, it is characterised in that including step：
1) under conditions of solvent, epoxy radicals end-blocking silicone oil and polyetheramine are added, under nitrogen protection, 6 is reacted in 80~85 DEG C
~8h, obtains the ternary polymerization silicon oil solution of low concentration；
2) the ternary polymerization silicon oil solution of low concentration is carried out into vacuum distillation, after removing partial solvent according to required concentration, immediately
Complex solvent is added, after stirring, terpolymer block silicone oil solution is obtained.
2. the method for claim 1, it is characterised in that step 1) in solvent for isopropanol or isopropanol with relatively
The mixed solvent of high boiling solvent, the of a relatively high boiling point solvent is dipropylene glycol methyl ether and/or propylene glycol monomethyl ether.
3. the method for claim 1, it is characterised in that step 1) the polyetheramine molecular weight is 2003g/mol.
4. the method for claim 1, it is characterised in that step 1) epoxy-capped silicone oil molecular weight for 8000~
17000g/mol。
5. the method as described in any one of Claims 1 to 4, it is characterised in that step 1) in epoxy-capped silicone oil and polyetheramine
Mol ratio be 1:2~2.2.
6. the method for claim 1, it is characterised in that step 2) in complex solvent be absolute ethyl alcohol, DPG
Methyl ether and dipropylene.
7. method as claimed in claim 6, it is characterised in that the complex solvent except absolute ethyl alcohol, dipropylene glycol methyl ether and
Beyond dipropylene, also including one or more combinations in propylene glycol monomethyl ether, propandiol butyl ether, DPG.
8. method as claimed in claims 6 or 7, it is characterised in that the absolute ethyl alcohol, dipropylene glycol methyl ether and DPG
The mass ratio of butyl ether is 6~8:2~3:1~2.
9. the method for claim 1, it is characterised in that the molecular weight for obtaining terpolymer block silicone oil solution is
12000~21000g/mol.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602873A (en) * | 2017-09-26 | 2018-01-19 | 上海应用技术大学 | A kind of hyperbranched silicone surfactant and preparation method thereof |
| CN109320725A (en) * | 2018-10-26 | 2019-02-12 | 纳派化学(上海)有限公司 | A kind of safe mixed solvent is used for block silicone oil synthesis technology |
| CN110205822A (en) * | 2019-07-15 | 2019-09-06 | 广东湛丰精细化工有限公司 | Dustless elastic silicone oil emulsion of one kind and preparation method thereof |
| CN110734549A (en) * | 2019-11-01 | 2020-01-31 | 湖州美伦纺织助剂有限公司 | ternary polymerization modified silicone oil and production process thereof |
| CN112480415A (en) * | 2020-11-27 | 2021-03-12 | 苏州联胜化学有限公司 | High-stability silicone oil for overflow machine and preparation method thereof |
| CN113004530A (en) * | 2021-04-12 | 2021-06-22 | 江苏尼美达科技有限公司 | Multi-component copolymer block silicone oil and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107602873A (en) * | 2017-09-26 | 2018-01-19 | 上海应用技术大学 | A kind of hyperbranched silicone surfactant and preparation method thereof |
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| CN110734549A (en) * | 2019-11-01 | 2020-01-31 | 湖州美伦纺织助剂有限公司 | ternary polymerization modified silicone oil and production process thereof |
| CN112480415A (en) * | 2020-11-27 | 2021-03-12 | 苏州联胜化学有限公司 | High-stability silicone oil for overflow machine and preparation method thereof |
| CN113004530A (en) * | 2021-04-12 | 2021-06-22 | 江苏尼美达科技有限公司 | Multi-component copolymer block silicone oil and preparation method thereof |
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Application publication date: 20170531 |