CN108341956A - A kind of preparation method of the universal imine modified block silicone softening agent of polyester-cotton blend - Google Patents
A kind of preparation method of the universal imine modified block silicone softening agent of polyester-cotton blend Download PDFInfo
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- CN108341956A CN108341956A CN201810096689.0A CN201810096689A CN108341956A CN 108341956 A CN108341956 A CN 108341956A CN 201810096689 A CN201810096689 A CN 201810096689A CN 108341956 A CN108341956 A CN 108341956A
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- polyester
- universal
- softening agent
- modified block
- cotton blend
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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
- C08G77/452—Block-or graft-polymers containing polysiloxane sequences containing nitrogen-containing 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
-
- 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
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- 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
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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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention relates to a kind of silicone softening agents, more particularly, to a kind of preparation method of the universal imine modified block silicone softening agent of polyester-cotton blend.It carries out according to the following steps：Raw material and proportioning → synthetic method and step.Products obtained therefrom molecular weight is high, viscosity is small, strong adsorption, versatile, can assign polyester fiber fabric fluffy, soft, plentiful feel effective on polyester fiber surface and penetrating into inside polyester fiber and form a film after baking；Modified silicone softening agent combines the Common advantages of both traditional block silicone oil and traditional amido silicon oil.
Description
Technical field
The present invention relates to a kind of silicone softening agents, more particularly, to a kind of universal imine modified block organosilicon of polyester-cotton blend
The preparation method of softening agent.
Background technology
In recent years, the type of block silicone oil is more and more, and using face is more and more wider.Just common block has on the market at present
The universal feel of fabric after machine silicone softener arranges is single-minded, washs bad on the cotton of good hand touch, and vice versa, is extremely difficult to high
Versatility, as dye-works workshop processes fabric variety diversification, it is desirable to which reaching polyester-cotton blend, general to generally require multiple organosilicons soft
Soft dose is used in compounding, and current numerous dye-works's forming machines have accomplished that pipeline, multiple silicone softening agents are used in conjunction with meaning
It and needs more head tanks, this is unfavorable for the utilization of spatial position and the management of factory formula, and multiple organosilicon flexibles
Effect after agent compounding is difficult often the advantages of embodying each independent softening agent.In order to reduce the arrangement cost of fabric, dye-works pair
Versatile organic silicone oil softening agent demand is obviously incremented by.
Invention content
Purpose of the present invention is to customer service the deficiencies in the prior art, provide one kind and solving traditional block silicone oil and traditional amino silicone
Oil assigns the unicity problem of polyester-cotton fabric performance；Synthesis technology is simple to operation, a kind of universal Asia of polyester-cotton blend of safety and environmental protection
The preparation method of amine modified block silicone softening agent.
To achieve the goals above, the present invention uses following technical scheme：
A kind of preparation method of the universal imine modified block silicone softening agent of polyester-cotton blend, carries out according to the following steps：
(1), raw material and proportioning：
90~110 parts of end hydrogen dimethyl silicone polymer, 7~13 parts of allyl polyoxy alkyl epoxy base ether, isopropanol 42~
52 parts, 5ppm~15ppm, the polyetheramine ED9005 that chloroplatinic acid (being calculated with platinum content) is the end total dosage of hydrogen dimethyl silicone polymer
~10 parts, 0.2~0.8 part of polyethyleneimine.
(2), synthetic method and step：
1) preparation of Epoxy-Terminated Polydimethylsiloxane：
End hydrogen dimethyl silicone polymer, allyl polyoxy alkyl epoxy base ether, isopropanol are added in reaction vessel, added
Chloroplatinic acid is added to 75~82 DEG C in heat, and insulation reaction 2~3 hours obtains Epoxy-Terminated Polydimethylsiloxane；
2) preparation of the universal imine modified block silicone softening agent of polyester-cotton blend：
1) the whole Epoxy-Terminated Polydimethylsiloxanes, polyetheramine ED-900, the polyethyleneimine that obtain in are added to
In reaction vessel, 78~82 DEG C are heated to, it is soft to obtain the universal imine modified block organosilicon of polyester-cotton blend for insulation reaction 5~6 hours
Soft dose.
Preferably, the number-average molecular weight of the end hydrogen dimethyl silicone polymer is one in 8000,10000,13000
Kind；The number-average molecular weight of the polyethyleneimine is 7000~10000.
Preferably, the number of raw material is all mass fraction.
A kind of preparation method of the universal imine modified block silicone softening agent of polyester-cotton blend produced by the present invention, products obtained therefrom
Molecular weight is high, viscosity is small, strong adsorption, versatile, can be effective on polyester fiber surface and penetrating into polyester fiber
Portion simultaneously forms a film after baking, and assigns polyester fiber fabric fluffy, soft, plentiful feel；Modified silicone softening agent knot
Close the Common advantages of both traditional block silicone oil and traditional amido silicon oil.
Description of the drawings
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.
Remarks：No. 1 curve is the infrared spectrum curve of Epoxy-Terminated Polydimethylsiloxane.
No. 2 curves are the infrared spectrum curve of the universal imine modified block silicone softening agent of polyester-cotton blend.
Specific implementation mode
Below by specific implementation mode, in conjunction with attached drawing, the present invention will be further described.
Embodiment 1：
1) the end hydrogen dimethyl silicone polymer by 100 grams average molecular weights for 8000,12.5 grams of allyl polyoxy alkyl rings
Oxygen ether, 45 grams of isopropanols are added in reaction vessel, are heated to 75 DEG C, are added 8 × 10-4Gram chloroplatinic acid, insulation reaction 2.5 are small
When, obtain Epoxy-Terminated Polydimethylsiloxane；
2) 1) the whole Epoxy-Terminated Polydimethylsiloxanes of middle gained, 9 gram polyetheramine ED-900s, 0.4 grams are divided equally
Son amount is added to for 8000 polyethyleneimine in reaction vessel, is heated to 80 DEG C, and it is logical to obtain polyester-cotton blend for insulation reaction 5.5 hours
With the imine modified block silicone softening agent of type.
Referring to attached drawing 1, it is the infrared spectrum of the universal imine modified block silicone softening agent of polyester-cotton blend in the present embodiment.
Two curves are compared, are 2963.49cm in wave number-1、2904.83cm-1、2967.24cm-1、2882.49cm-1Place is-CH3It is anti-
Symmetrical stretching vibration peak and symmetrical stretching vibration peak are 970~1100cm in wave number-1Place is the stretching vibration peak of Si-O keys,
Wave number is 1446.89cm-1、1412.85cm-1、1466.84cm-1、1410.30cm-1Place is Si-CH3Upper-CH3Symmetric deformation
Vibration peak, in wave number 1256.69cm-1、1259.72cm-1Place is the absorption peak of C-O-C, in 600~960cm of wave number-1Place is Si-
The stretching vibration peak of C keys, two curves of comparison find out modified block silicone oil curve in 1378.84cm-1Locate mostly an absorption peak,
The new absorption peak occurred is the characteristic absorption peak of imine group, shows that target product successfully obtains.
Embodiment 2：
1) the end hydrogen dimethyl silicone polymer by 105 grams average molecular weights for 10000,10.5 grams of allyl polyoxy alkyl rings
Oxygen ether, 48 grams of isopropanols are added in reaction vessel, are heated to 78 DEG C, are added 9.5 × 10-4Gram chloroplatinic acid, insulation reaction 2 are small
When, obtain Epoxy-Terminated Polydimethylsiloxane；
2) 1) the whole Epoxy-Terminated Polydimethylsiloxanes of middle gained, 8.6 gram polyetheramine ED-900s, 0.55 grams is equal
The polyethyleneimine that molecular weight is 9000 is added in reaction vessel, is heated to 81 DEG C, and it is logical to obtain polyester-cotton blend for insulation reaction 5 hours
With the imine modified block silicone softening agent of type.
Referring to attached drawing 2, it is the infrared spectrum of the universal imine modified block silicone softening agent of polyester-cotton blend in the present embodiment.
Two curves are compared, are 2962.85cm in wave number-1、2904.68cm-1、2962.85cm-1、2904.44cm-1Place is-CH3It is anti-
Symmetrical stretching vibration peak and symmetrical stretching vibration peak are 990~1100cm in wave number-1Place is the stretching vibration peak of Si-O keys,
Wave number is 1412.49cm-1、1466.96cm-1、1411.61cm-1, place be Si-CH3Upper-CH3Symmetrical deformation vibration peak, in wave
Number 1256.99cm-1、1256.61cm-1Place is the absorption peak of C-O-C, in 600~960cm of wave number-1Place is that the flexible of Si-C keys shakes
Dynamic peak, two curves of comparison find out modified block silicone oil curve in 1378.78cm-1The more absorption peaks in place, appearance it is new
Absorption peak is the characteristic absorption peak of imine group, shows that target product successfully obtains.
Embodiment 3：
1) the end hydrogen dimethyl silicone polymer by 110 grams average molecular weights for 13000,7.5 grams of allyl polyoxy alkyl rings
Oxygen ether, 50 grams of isopropanols are added in reaction vessel, are heated to 81 DEG C, are added 11 × 10-4Gram chloroplatinic acid, insulation reaction 3 are small
When, obtain Epoxy-Terminated Polydimethylsiloxane；
2) 1) the whole Epoxy-Terminated Polydimethylsiloxanes of middle gained, 7.2 gram polyetheramine ED-900s, 0.65 grams is equal
Molecular weight is that 10000 polyethyleneimines are added in reaction vessel, is heated to 80 DEG C, it is general to obtain polyester-cotton blend for insulation reaction 6 hours
The imine modified block silicone softening agent of type.
Referring to attached drawing 3, it is the infrared spectrum of the universal imine modified block silicone softening agent of polyester-cotton blend in the present embodiment.
Two curves are compared, are 2962.84cm in wave number-1、2901.80cm-1、2965.71cm-1、2901.29cm-1Place is-CH3It is anti-
Symmetrical stretching vibration peak and symmetrical stretching vibration peak are 950~1150cm in wave number-1Place is the stretching vibration peak of Si-O keys,
Wave number is 1447.55cm-1、1412.35cm-1、1466.64cm-1、1411.74cm-1Place is Si-CH3Upper-CH3Symmetric deformation
Vibration peak, in wave number 1258.21cm-1、1258.78cm-1Place is the absorption peak of C-O-C, in 700~870cm of wave number-1Place is Si-
The stretching vibration peak of C keys, two curves of comparison find out modified block silicone oil curve in 1340.98cm-1Locate mostly an absorption peak,
The new absorption peak occurred is the characteristic absorption peak of imine group, shows that target product successfully obtains.
Polyester-cotton blend generic imine modified block silicone softening agent application finishing technique：
1. polyester-cotton blend generic imine modified block organosilicon flexible agent emulsion is prepared：
Note：The number of raw material is all mass fraction
2. finishing technique：
Fabric used：It washs woven fabric, cotton woven fabric, wash looped fabric, cotton looped fabric.
Finishing technique flow：Pad working solution (the universal amide modifications block organosilicon flexible agent emulsion 20g/L of polyester-cotton blend,
Pick-up 80%) → bake and (wash looped fabric, wash 190 DEG C × 40s of woven fabric, 170 DEG C cotton looped fabric, cotton woven fabric × 40s) →
Moisture regain 24 hours → test, 3. application performance tests：
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, take total score.
Discoloration：The color change of front and back fabric is arranged with the test of computer color measurement and color match instrument.
Crock fastness：With reference to GB/T3920-1997《Textile color stability tests colour fastness to rubbing》It is tested.
Washing fastness：With reference to GB/T3921.1-1997《Textile color stability tests color fastness to washing》It is tested.
The results are shown in Table 1 for the universal imine modified block silicone softening agent application performance test of polyester-cotton blend of the present invention：
The universal imine modified block silicone softening agent application performance test result of 1 polyester-cotton blend of table
As can be seen from the above table, the fabric after the universal imine modified block silicone softening agent of polyester-cotton blend of the present invention arranges
Fluffy flexibility is better than commercially available block silicone oil, and it is small to decline degree after washing；It is smaller on the influence of fabric dry and wet crock fastness, and color
It is lower.
Claims (3)
1. a kind of preparation method of the universal imine modified block silicone softening agent of polyester-cotton blend, it is characterised in that according to the following steps into
Row：
(1), raw material and proportioning：
Hold 90~110 parts of hydrogen dimethyl silicone polymer, 7~13 parts of allyl polyoxy alkyl epoxy base ether, 42~52 parts of isopropanol,
Chloroplatinic acid (being calculated with platinum content) is the 5ppm~15ppm for holding the total dosage of hydrogen dimethyl silicone polymer, polyetheramine ED9005~10
Part, 0.2~0.8 part of polyethyleneimine.
(2), synthetic method and step：
1) preparation of Epoxy-Terminated Polydimethylsiloxane：
End hydrogen dimethyl silicone polymer, allyl polyoxy alkyl epoxy base ether, isopropanol are added in reaction vessel, are heated to
75~82 DEG C, chloroplatinic acid is added, insulation reaction 2~3 hours obtains Epoxy-Terminated Polydimethylsiloxane；
2) preparation of the universal imine modified block silicone softening agent of polyester-cotton blend：
1) the whole Epoxy-Terminated Polydimethylsiloxanes, polyetheramine ED-900, the polyethyleneimine that obtain in are added to reaction
In container, 78~82 DEG C are heated to, insulation reaction 5~6 hours obtains the universal imine modified block organosilicon flexible of polyester-cotton blend
Agent.
2. a kind of preparation method of the universal imine modified block silicone softening agent of polyester-cotton blend according to claim 1,
It is characterized in that：The number-average molecular weight of the end hydrogen dimethyl silicone polymer is one kind in 8000,10000,13000；It is described poly-
The number-average molecular weight of aziridine is 7000~10000.
3. a kind of preparation method of the universal imine modified block silicone softening agent of polyester-cotton blend according to claim 1,
It is characterized in that：The number of raw material is all mass fraction.
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| CN201810096689.0A CN108341956B (en) | 2018-01-31 | 2018-01-31 | Preparation method of universal type imine modified block organosilicon softener for polyester cotton |
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|---|---|---|---|
| CN201810096689.0A CN108341956B (en) | 2018-01-31 | 2018-01-31 | Preparation method of universal type imine modified block organosilicon softener for polyester cotton |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019114493A1 (en) * | 2017-12-14 | 2019-06-20 | Basf Se | Copolymer of polyalkylenimine and polysiloxane and compositions con-taining the same |
| CN111576036A (en) * | 2020-05-20 | 2020-08-25 | 浙江海明实业有限公司 | Nano antifouling, antibacterial and breathable environment-friendly fabric and preparation process thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2019114493A1 (en) * | 2017-12-14 | 2019-06-20 | Basf Se | Copolymer of polyalkylenimine and polysiloxane and compositions con-taining the same |
| CN111576036A (en) * | 2020-05-20 | 2020-08-25 | 浙江海明实业有限公司 | Nano antifouling, antibacterial and breathable environment-friendly fabric and preparation process thereof |
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| Publication number | Publication date |
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| CN108341956B (en) | 2021-03-05 |
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