CN110372868A - A kind of preparation method of the low discoloration piperazinyl sealing end polyether-modified block silicone oil of esteramides - Google Patents
A kind of preparation method of the low discoloration piperazinyl sealing end polyether-modified block silicone oil of esteramides Download PDFInfo
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- CN110372868A CN110372868A CN201910676022.2A CN201910676022A CN110372868A CN 110372868 A CN110372868 A CN 110372868A CN 201910676022 A CN201910676022 A CN 201910676022A CN 110372868 A CN110372868 A CN 110372868A
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- esteramides
- silicone oil
- piperazinyl
- piperazine
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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
-
- 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
- D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
-
- 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
- D06M2101/34—Polyamides
-
- 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 textile auxiliary field more particularly to a kind of preparation methods of the low discoloration piperazinyl sealing end polyether-modified block silicone oil of esteramides, are made by N- aminoethyl piperazine, epoxy sealing head agent, esteramides polyethers, end epoxy silicon oil, isopropanol for raw material.The arrangement of nylon fabric will be used for after the silicone oil emulsification, fabric after processing not only to have preferable soft, smooth feel, but also low discoloration.The present invention introduces piperazine, polyethers and amide group in the main chain of silicone oil, and traditional block silicone oil is overcome to arrange the defect that adsorption rate is low, discoloration is big, hydrophily is poor and feel is undesirable for nylon fabric.
Description
Technical field
The present invention relates to a kind of textile auxiliary fields, more particularly, to a kind of preparation method of low siliceous degreaser of bubble.
Background technique
In recent years, amino-polyether block silicone oil is quickly grown in textile industry, but main still to hold epoxy silicon oil and ED
Series polyether amine, D series polyether amine and the reaction synthesis of polyethylene polyamine series amine, can assign dacron, cotton after arranging and knit
The excellent soft feel of object, polyester-cotton fabric and retain the certain hydrophily of fabric, but it is past through its nylon fabric after arranging
Poor toward there is hygroscopicity, dress is sultry, and ideal feel is not achieved, and wearability substantially reduces, and the fabric after arrangement is easy
Discoloration.
Nylon fiber belongs to long filament and rigidity is larger, and woven fabric is often more stiff, and the fabric after arrangement will have soft
The performances such as soft, smooth generally require multiple silicone softening agent compoundings and arrange, and pipeline has been accomplished by current numerous dye-works,
Multiple silicone softening agents, which are used in conjunction with, is intended to more storage tank equipments, this is unfavorable for the utilization and production of spatial position
The management of formula greatly improves the production cost of dye-works.In order to reduce production cost, better economic benefit, dye-works pair are obtained
High sexual valence, high performance silicone oil demand are incremented by obvious.
Summary of the invention
Object of the present invention is to customer service the deficiencies in the prior art, providing a kind of will be used for the whole of nylon fabric after the silicone oil emulsification
Reason, fabric after processing not only has preferable soft, smooth feel, but also the low discoloration piperazinyl of low discoloration blocks esteramides
The preparation method of polyether-modified block silicone oil.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of preparation method of the low discoloration piperazinyl sealing end polyether-modified block silicone oil of esteramides, it is characterised in that by following
Step carries out:
(1), raw material proportioning:
Following raw material is matched by weight:
5.5 parts~8.5 parts of N- aminoethyl piperazine, 7 parts~9 parts of epoxy sealing head agent, end 200 parts of epoxy silicon oil~400 parts, ester
9.5 parts~12.5 parts of amide polyethers, 90 parts~120 parts of isopropanol.
(2), preparation step:
1) preparation of both-end piperazine end socket；
5.5 parts~8.5 parts of N- aminoethyl piperazine are added in reaction vessel, 7 parts~9 parts suction high positions of epoxy sealing head agent
Slot, reaction vessel are warming up to 60 DEG C~90 DEG C, and epoxy sealing head agent is added dropwise, is added dropwise to complete rear insulation reaction 2~4 hours, are made double
Hold piperazine end socket；
2) preparation of the low discoloration piperazinyl sealing end polyether-modified block silicone oil of esteramides；
200 parts~400 parts of end epoxy silicon oil, 9.5 parts~12.5 parts of esteramides polyethers, 90 parts~120 parts of isopropanol are added
Enter into reaction vessel, after being heated to 78 DEG C~83 DEG C, insulation reaction 8~10 hours, is added in 1) and obtains into reaction vessel
Whole both-end piperazine end sockets the required low discoloration piperazine of the present invention is prepared at 78 DEG C~83 DEG C, insulation reaction 5~8 hours
Piperazine base blocks the polyether-modified block silicone oil of esteramides, and general structure is as follows；
It is 4~13, b is 3~6 that n, which is 130~197, a, in formula.
Preferably, the number-average molecular weight of the end epoxy silicon oil is one of 10000,13000,15000.
Due to the application of the above technical scheme, the present invention has the advantage that
Piperazine, polyethers and amide group are introduced simultaneously in silicone oil main chain of the present invention, and the introducing of piperazine group not only can be with
Improve the flexibility of finish fabric, and the discoloration of fabric is small, introducings of polyether group can make the fabric after arranging with compared with
Good hydrophily, the introducing of amide group improve adsorption rate of the silicone oil in nylon fabric, and silicone oil of the present invention overcomes tradition embedding
Section silicone oil arranges the defect that discoloration is big, hydrophily is poor, adsorption rate is low and feel is undesirable, products obtained therefrom molecule for nylon fabric
Amount is high, viscosity is small, strong adsorption, can effective on nylon fabric surface and penetrate into inside nylon fabric and after baking at
Film, assigns soft nylon fabric, smooth feel and preferable hydrophilicity and fabric discoloration is small；Modified block silicone oil solution
Traditional block silicone oil of having determined assigns nylon fabric performance undesirable problem；Synthesis technology is simple to operation, safety and environmental protection.
Specific embodiment
Below by specific embodiment, the present invention will be further described.
Embodiment 1:
1) 55 grams of N- aminoethyl piperazines are added in reaction vessel, 70 grams of epoxy sealing head agent are pumped into head tank, reaction appearance
Device is warming up to 65 DEG C, and epoxy sealing head agent is added dropwise, is added dropwise to complete rear insulation reaction 2 hours, and both-end piperazine end socket is made；
It 2) is 10000 end epoxy silicon oils, 95 grams of esteramides polyethers, 900 grams of isopropanol additions by 2000 grams average molecular weights
Into reaction vessel, after being heated to 78 DEG C, insulation reaction 8 hours, be added into reaction vessel 1) obtained in whole both-end piperazine
Piperazine end socket is prepared the required low discoloration piperazinyl sealing end esteramides polyethers of the present invention and changes at 78 DEG C, insulation reaction 5 hours
Property block silicone oil.
Embodiment 2:
1) 70 grams of N- aminoethyl piperazines are added in reaction vessel, 80 grams of epoxy sealing head agent are pumped into head tank, reaction appearance
Device is warming up to 70 DEG C, and epoxy sealing head agent is added dropwise, is added dropwise to complete rear insulation reaction 3 hours, and both-end piperazine end socket is made；
2) by 3000 grams average molecular weights be 13000 end epoxy silicon oils, 105 grams of esteramides polyethers, 1000 grams of isopropanol plus
Enter into reaction vessel, after being heated to 80 DEG C, insulation reaction 9 hours, be added into reaction vessel 1) obtained in whole both-end
The required low discoloration piperazinyl sealing end esteramides polyethers of the present invention is prepared at 80 DEG C, insulation reaction 6 hours in piperazine end socket
Modified block silicone oil.
Embodiment 3:
1) 80 grams of N- aminoethyl piperazines are added in reaction vessel, 90 grams of epoxy sealing head agent are pumped into head tank, reaction appearance
Device is warming up to 85 DEG C, and epoxy sealing head agent is added dropwise, is added dropwise to complete rear insulation reaction 4 hours, and both-end piperazine end socket is made；
2) by 3500 grams average molecular weights be 15000 end epoxy silicon oils, 115 grams of esteramides polyethers, 1100 grams of isopropanol plus
Enter into reaction vessel, after being heated to 82 DEG C, insulation reaction 10 hours, be added into reaction vessel 1) obtained in whole both-end
The required low discoloration piperazinyl sealing end esteramides polyethers of the present invention is prepared at 82 DEG C, insulation reaction 8 hours in piperazine end socket
Modified block silicone oil.
Low discoloration piperazinyl blocks the polyether-modified block silicone oil application finishing technique of esteramides:
1. the polyether-modified block silicone oil lotion of low discoloration piperazinyl sealing end esteramides is prepared
2. finishing technique
Fabric used: nylon woven fabric.
Finishing technique process: padding working solution, (low discoloration piperazinyl blocks the polyether-modified block silicone oil lotion of esteramides
40g/L, pick-up 60%~70%) → bake (195 DEG C × 40s~60s) → resurgence 24 hours → test
3. application performance test
Smooth property evaluation: 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 for arranging front and back fabric is tested with computer color measurement and color match instrument.
Crock fastness: it is tested with reference to GB/T3920-1997 " textile color stability test colour fastness to rubbing ".
Low discoloration piperazinyl of the invention blocks the polyether-modified block silicone oil application performance test result of esteramides such as 1 institute of table
Show:
The low discoloration piperazinyl of table 1 blocks the polyether-modified block silicone oil application performance test result of esteramides
As can be seen from the above table, after the polyether-modified block silicone oil of the low discoloration piperazinyl sealing end esteramides of the present invention arranges
The smooth property of nylon fabric is better than commercially available block silicone oil, smaller on the influence of fabric dry and wet crock fastness, and discoloration is low.
Claims (2)
1. a kind of preparation method of the low discoloration piperazinyl sealing end polyether-modified block silicone oil of esteramides, it is characterised in that press following step
It is rapid to carry out:
(1), raw material proportioning:
Following raw material is matched by weight:
5.5 parts~8.5 parts of N- aminoethyl piperazine, 7 parts~9 parts of epoxy sealing head agent, end 200 parts of epoxy silicon oil~400 parts, esteramides
9.5 parts~12.5 parts of polyethers, 90 parts~120 parts of isopropanol.
(2), preparation step:
1) preparation of both-end piperazine end socket；
5.5 parts~8.5 parts of N- aminoethyl piperazine are added in reaction vessel, 7 parts~9 parts suction head tanks of epoxy sealing head agent,
Reaction vessel is warming up to 60 DEG C~90 DEG C, and epoxy sealing head agent is added dropwise, is added dropwise to complete rear insulation reaction 2~4 hours, and both-end piperazine is made
Piperazine end socket；
2) preparation of the low discoloration piperazinyl sealing end polyether-modified block silicone oil of esteramides；
200 parts~400 parts of the epoxy silicon oil in end, 9.5 parts~12.5 parts of esteramides polyethers, 90 parts~120 parts of isopropanol are added to
In reaction vessel, after being heated to 78 DEG C~83 DEG C, insulation reaction 8~10 hours, be added into reaction vessel 1) obtained in it is complete
The required low discoloration piperazinyl of the present invention is prepared at 78 DEG C~83 DEG C, insulation reaction 5~8 hours in portion's both-end piperazine end socket
The polyether-modified block silicone oil of esteramides is blocked, general structure is as follows；
It is 4~13, b is 3~6 that n, which is 130~197, a, in formula.
2. a kind of preparation side of low discoloration piperazinyl sealing end polyether-modified block silicone oil of esteramides according to claim 1
Method, it is characterised in that: the number-average molecular weight of the end epoxy silicon oil is one of 10000,13000,15000.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910676022.2A CN110372868B (en) | 2019-07-25 | 2019-07-25 | Preparation method of low-discoloration piperazinyl terminated ester amide polyether modified block silicone oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910676022.2A CN110372868B (en) | 2019-07-25 | 2019-07-25 | Preparation method of low-discoloration piperazinyl terminated ester amide polyether modified block silicone oil |
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| Publication Number | Publication Date |
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| CN110372868A true CN110372868A (en) | 2019-10-25 |
| CN110372868B CN110372868B (en) | 2021-07-30 |
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Cited By (5)
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| CN111393654A (en) * | 2020-04-29 | 2020-07-10 | 杭州美高华颐化工有限公司 | Preparation method of multifunctional nylon block silicone oil |
| CN112680973A (en) * | 2020-12-28 | 2021-04-20 | 绍兴海成化工有限公司 | In-cylinder silicone oil and preparation method thereof |
| CN113373696A (en) * | 2021-06-18 | 2021-09-10 | 广东宏昊化工有限公司 | Softening agent for bamboo fiber fabric and preparation method thereof |
| CN115521465A (en) * | 2022-10-21 | 2022-12-27 | 常州市中策纺织助剂有限公司 | Preparation method of low-yellowing organic silicon softening agent |
| CN116396464A (en) * | 2023-05-10 | 2023-07-07 | 杭州美高华颐化工有限公司 | Preparation method of isophorone diisocyanate blocked block silicone oil |
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| CN113373696A (en) * | 2021-06-18 | 2021-09-10 | 广东宏昊化工有限公司 | Softening agent for bamboo fiber fabric and preparation method thereof |
| CN115521465A (en) * | 2022-10-21 | 2022-12-27 | 常州市中策纺织助剂有限公司 | Preparation method of low-yellowing organic silicon softening agent |
| CN116396464A (en) * | 2023-05-10 | 2023-07-07 | 杭州美高华颐化工有限公司 | Preparation method of isophorone diisocyanate blocked block silicone oil |
| CN116396464B (en) * | 2023-05-10 | 2024-04-16 | 杭州美高华颐化工有限公司 | Preparation method of isophorone diisocyanate blocked block silicone oil |
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