CN108384016A - A kind of preparation method of side chain type polysiloxane - Google Patents
A kind of preparation method of side chain type polysiloxane Download PDFInfo
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- CN108384016A CN108384016A CN201810291439.2A CN201810291439A CN108384016A CN 108384016 A CN108384016 A CN 108384016A CN 201810291439 A CN201810291439 A CN 201810291439A CN 108384016 A CN108384016 A CN 108384016A
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- parts
- side chain
- chain type
- type polysiloxane
- end ring
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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
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
- C08G77/388—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon containing nitrogen
-
- 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
- D06M2200/35—Abrasion, pilling or fibrillation resistance
-
- 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)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Silicon Polymers (AREA)
Abstract
The present invention relates to a kind of organosiloxanes, more particularly, to a kind of preparation method of side chain type polysiloxane.Including following raw material, matched by weight：95~110 parts, N, N, N, N of end ring oxygen dimethyl silicone polymer, 1~3 part of N five methyl diethylentriamines, 3~6 parts of polyethyleneglycol diglycidylether, 3~6 parts of lauric acid, 80~100 parts of ethylene glycol monobutyl ether.Quaternary ammonium group content is high in molecular structure, hydrophily and excellent antistatic property.
Description
Technical field
The present invention relates to a kind of organosiloxanes, more particularly, to a kind of preparation method of side chain type polysiloxane.
Background technology
The synthetic technology of quaternary ammonium type polyorganosiloxane compounds is gradually ripe, and many researchers use α, ω-bis-
End ring oxygen polydimethylsiloxane is reacted with tertiary amine compounds under acid catalysis, generates α, the bis- quaternary ammonium group poly organos of ω-
Alkane.And applied on cotton fabric, fabric can not only be made to obtain excellent hydrophily, and there is preferable whiteness and softness
Property.But the block silicone oil of this type, in chemical fiber plus material, the hydrophilic effect especially on dacron is poor.This is because terylene is fine
Lack reactive group in dimension structure, silicone segments are unordered in the arrangement of fiber surface, and hydrophilic quaternary groups is caused to be had
Machine silicon segment coats, and hydrophilicity declines.So making with bath with antistatic agent frequently with organic silicone finishing agent in actual production
With electrostatic problem caused by fabric hydrophilic difference after being arranged with reduction.But the use of antistatic agent can cause fabric softness
Decline.
Invention content
Purpose of the present invention is to customer service the deficiencies in the prior art, a kind of side chain type hydrophily is provided and antistatic property is excellent
A kind of preparation method of side chain type polysiloxane.
To achieve the goals above, the present invention uses following technical scheme：
A kind of side chain type polysiloxane, including following raw material, are matched by weight：
95~110 parts, N, N, N, N of end ring oxygen dimethyl silicone polymer, 1~3 part of N- five methyl diethylentriamines, poly- second
3~6 parts of Hexanediol diglycidyl ether, 3~6 parts of lauric acid, 80~100 parts of ethylene glycol monobutyl ether.
A kind of preparation method of side chain type polysiloxane, is synthesized as follows method and step：
By end ring oxygen dimethyl silicone polymer, N, N, N, N, N- five methyl diethylentriamines, lauric acid and ethylene glycol list
Butyl ether is added in the reaction vessel equipped with condensation reflux unit, is heated to 110~125 DEG C, and poly- second two is added after keeping the temperature 4~6h
Alcohol diglycidyl ether continues 1~2h of heat preservation at 110~125 DEG C, is cooled to 50 DEG C with bottom discharge, obtains target product,
General structure is：
Wherein：130≤n≤170,6≤m≤10,5≤p≤10.
Preferably, the end ring oxygen dimethyl silicone polymer molecular weight is one kind in 10000,12000,13000, institute
It is one kind in 400,600 to state polyethyleneglycol diglycidylether molecular weight.
The present invention uses N, N, N, and N, N- five methyl diethylentriamines are three-functionality-degree, with end ring oxygen polydimethylsiloxanes
After alkane reaction, quaternary ammonium group content is high in molecular structure, hydrophily and excellent antistatic property.Poly- second is grafted on strand main chain
Hexanediol diglycidyl ether functional side so that during baking arrangement, hydrophobic polysiloxane segment is adsorbed on fiber table
Face, hydrophilic polyglycol segment extend in outside, compensate for the hydrophilicity caused by quaternary ammonium group is wrapped by and decline, make whole
Soft fabric performance preferably simultaneously, has excellent hydrophily and antistatic property after reason.And the unreacted ring of side chain terminal
Oxygen groups play the role of crosslinked, the washability of fabric after raising arranges during arranging.
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.
Specific implementation mode
Below by specific implementation mode, in conjunction with attached drawing, the present invention will be further described.
Embodiment 1：
By 100 parts of 10000 end ring oxygen dimethyl silicone polymers of molecular weight, 2 parts of N, N, N, N, N- pentamethyls diethylidene three
Amine, 4 parts of lauric acid and 90 parts of ethylene glycol monobutyl ethers are added in the reaction vessel equipped with condensation reflux unit, are heated to 120 DEG C,
The polyethyleneglycol diglycidylether of 4 parts of molecular weight 400 is added after heat preservation 4h, continues to keep the temperature 1h at 110 DEG C, is cooled to 50 DEG C
With bottom discharge, target product is obtained,
Referring to attached drawing 1, it is the infrared spectrum of hyperbranched silicone softening agent in the present embodiment.In 1258.17cm-1、
862.48cm-1And 1000cm-1~1130cm-1There are three absorption peaks in place, is Si-CH in silicone segments3、Si-OCH2CH3With
The characteristic absorption peak of Si-O-Si, 910cm-1The weak absorbing peak that vicinity occurs is the characteristic absorption peak of residual epoxy group, is shown
Target product successfully obtains.
Embodiment 2：
By 100 parts of 13000 end ring oxygen dimethyl silicone polymers of molecular weight, 1.5 parts of N, N, N, N, N- pentamethyl diethylidenes
Triamine, 3 parts of lauric acid and 88 parts of ethylene glycol monobutyl ethers are added in the reaction vessel equipped with condensation reflux unit, are heated to 125
DEG C, the polyethyleneglycol diglycidylether of 3 parts of molecular weight 600 of addition after 6h is kept the temperature, continues to keep the temperature 2h at 115 DEG C, be cooled to
50 DEG C, with bottom discharge, obtain target product；
Referring to attached drawing 2, it is the infrared spectrum of hyperbranched silicone softening agent in the present embodiment.In 1258.08cm-1、
862.41cm-1And 1000cm-1~1130cm-1There are three absorption peaks in place, is Si-CH in silicone segments3、Si-OCH2CH3With
The characteristic absorption peak of Si-O-Si, 910cm-1The weak absorbing peak that vicinity occurs is the characteristic absorption peak of residual epoxy group, is shown
Target product successfully obtains.
Embodiment 3：
By 100 parts of 10000 end ring oxygen dimethyl silicone polymers of molecular weight, 3 parts of N, N, N, N, N- pentamethyls diethylidene three
Amine, 6 parts of lauric acid and 95 parts of ethylene glycol monobutyl ethers are added in the reaction vessel equipped with condensation reflux unit, are heated to 115 DEG C,
The polyethyleneglycol diglycidylether of 4 parts of molecular weight 600 is added after heat preservation 5h, continues to keep the temperature 2h at 120 DEG C, is cooled to 50 DEG C
With bottom discharge, target product is obtained,
Referring to attached drawing 3, it is the infrared spectrum of side chain functionalities polysiloxane in the present embodiment.1258.25cm-1、
862.49cm-1And 1000cm-1~1130cm-1There are three absorption peaks in place, is Si-CH in silicone segments3、Si-OCH2CH3With
The characteristic absorption peak of Si-O-Si, 910cm-1The weak absorbing peak that vicinity occurs is the characteristic absorption peak of residual epoxy group, is shown
Target product successfully obtains.
Side chain type polysiloxane application finishing technique：
1. lotion is prepared
2. finishing technique
Fabric used：White washs woven fabric.
Finishing technique flow：Working solution (lotion 30g/L, pick-up 60%) → baking (195 DEG C × 30s) → is padded to get damp again
For 24 hours → test
3. application performance test
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.
Hydrophily：With reference to AATCC 79-2010《Bleaching textiles absorbability》It is tested.Antistatic property：GB/
T12703.1-2008《The evaluation part 1 of textile antistatic property:Electrostatic pressure half-life period》
The results are shown in Table 1 for the side chain functionalities polysiloxane application performance test of the present invention：
1 side chain type polysiloxane application performance test result of table
As seen from the above table, through side chain type polysiloxane of the present invention arrangement after fabric softness it is excellent, hydrophily and
Antistatic property performance is obviously improved.
Claims (3)
1. a kind of side chain type polysiloxane, it is characterised in that：Including following raw material, matched by weight：
95~110 parts, N, N, N, N of end ring oxygen dimethyl silicone polymer, 1~3 part of N- five methyl diethylentriamines, polyethylene glycol
3~6 parts of diglycidyl ether, 3~6 parts of lauric acid, 80~100 parts of ethylene glycol monobutyl ether.
2. a kind of preparation method of side chain type polysiloxane according to right 1, it is characterised in that：The side of being synthesized as follows
Method and step：
By end ring oxygen dimethyl silicone polymer, N, N, N, N, N- five methyl diethylentriamines, lauric acid and ethylene glycol monobutyl ether
It is added in the reaction vessel equipped with condensation reflux unit, is heated to 110~125 DEG C, polyethylene glycol two is added after keeping the temperature 4~6h
Glycidol ether continues 1~2h of heat preservation at 110~125 DEG C, is cooled to 50 DEG C with bottom discharge, obtains target product, structure
General formula is：
Wherein：130≤n≤170,6≤m≤10,5≤p≤10.
3. a kind of preparation method of side chain type polysiloxane according to claim 2, which is characterized in that the end ring
Oxygen dimethyl silicone polymer molecular weight is one kind in 10000,12000,13000, the polyethyleneglycol diglycidylether point
Son amount is one kind in 400,600.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810291439.2A CN108384016A (en) | 2018-04-03 | 2018-04-03 | A kind of preparation method of side chain type polysiloxane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810291439.2A CN108384016A (en) | 2018-04-03 | 2018-04-03 | A kind of preparation method of side chain type polysiloxane |
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| Publication Number | Publication Date |
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| CN108384016A true CN108384016A (en) | 2018-08-10 |
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| CN201810291439.2A Pending CN108384016A (en) | 2018-04-03 | 2018-04-03 | A kind of preparation method of side chain type polysiloxane |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111280175A (en) * | 2020-03-06 | 2020-06-16 | 威海诺葳信和新材料有限公司 | Multi-point quaternary ammonium salt modified organic silicon copolymer type antibacterial agent and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002066559A1 (en) * | 2001-02-20 | 2002-08-29 | Crompton Corporation | Organopolysiloxane composition, method of making emulsion-forming organopolysiloxane composition and method of treating textile fiber or fabric |
| CN103113590A (en) * | 2013-01-16 | 2013-05-22 | 杭州美高华颐化工有限公司 | Quaternary ammonium base organopolysiloxane high-molecular compound and preparation method and application thereof |
-
2018
- 2018-04-03 CN CN201810291439.2A patent/CN108384016A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002066559A1 (en) * | 2001-02-20 | 2002-08-29 | Crompton Corporation | Organopolysiloxane composition, method of making emulsion-forming organopolysiloxane composition and method of treating textile fiber or fabric |
| CN103113590A (en) * | 2013-01-16 | 2013-05-22 | 杭州美高华颐化工有限公司 | Quaternary ammonium base organopolysiloxane high-molecular compound and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 陈焜等: "《无溶剂亲水嵌段硅油M-5175的合成及应用》", 《印染》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111280175A (en) * | 2020-03-06 | 2020-06-16 | 威海诺葳信和新材料有限公司 | Multi-point quaternary ammonium salt modified organic silicon copolymer type antibacterial agent and preparation method thereof |
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Application publication date: 20180810 |