CN101525438A - Method for preparing polyether modified epoxy/amino silicone oil - Google Patents
Method for preparing polyether modified epoxy/amino silicone oil Download PDFInfo
- Publication number
- CN101525438A CN101525438A CN200910029295A CN200910029295A CN101525438A CN 101525438 A CN101525438 A CN 101525438A CN 200910029295 A CN200910029295 A CN 200910029295A CN 200910029295 A CN200910029295 A CN 200910029295A CN 101525438 A CN101525438 A CN 101525438A
- Authority
- CN
- China
- Prior art keywords
- silicon oil
- modified epoxy
- polyether modified
- polyether
- amido silicon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention relates to a method for preparing polyether modified epoxy/amino silicone oil, and particularly belongs to the technical field of textile chemical industry. Hydrogen-containing amino silicone oil, alkenyl epoxy compounds, active polyether and isopropanol are added in a reaction kettle, nitrogen is introduced, and the mixture is stirred and heated; a catalyst is dropped in the reaction kettle for reaction, then the reaction kettle is vacuumized, and the isopropanol is removed to obtain a finished product. By the preparation method, common amino silicone oil can be directly modified, reaction steps are simple, and reaction conditions are mild and easy to operate; a finished textile retains good quality of soft and smooth hand touch and has the characteristic of good hydrophilicity; in the use process, oil is not easy to float, the yellowing property is reduced, and the wash resistance is increased.
Description
Technical field
The present invention relates to a kind of preparation method of polyether modified epoxy/amido silicon oil, specifically belong to technical field of textile chemical engineering.
Background technology
People to the requirement of clothes not only require the fabric dress comfortable, good water absorbability and ventilation property are arranged, also pursue fabric sofetening, smooth, elegant style simultaneously.Therefore softening more and more is subject to people's attention, and the major objective of softening is to obtain feel and convenient weaving processing preferably and improve wear behavior.Softening agent is the important auxiliary agent of natural fiber and synthetic fabrics aftertreatment.Weaving mostly is silicone based softening agent greatly with softening agent, amino-modified silicone oil is a kind of positively charged ion silicone oil, with fiber associativity is arranged, and is the important fabric post-treatment agent of a class, can improve the feel of fabric, make it to have softness, level and smooth, bullet very, crease-resistant, antistatic property etc., and toxicological harmless is widely used in the soft function arrangement of textiles, itself and the crosslinked film forming of fabric, but this film water dissolubility is poor, and the fabric hydrophobicity after the arrangement is stronger, and washing fastness is poor; Simultaneously because amino existence, the fabric generation xanthochromia after oxidation makes processing easily under high temperature and the irradiate light, so it should not be used for the softening of light fabric.Modification to amino-silicone oil softening agent at present mainly contains cation quaternary ammonium salt modification, nonionic polyoxyalkylene modification, and the product after the modification can both suppress the xanthochromia of amido silicon oil to a certain extent, but the flexibility of this amido silicon oil is descended to some extent.If in amido silicon oil, introduce epoxy group(ing) and polyether segment, the silicone oil wetting ability is increased, and after the carboxyl reaction in epoxy group(ing) and the fabric, washing fastness further strengthen.
Patent CN1927910A discloses a kind of preparation method of amino/epoxy co-modified hydrophilic silicone oil, this modified silicon oil is to adopt silicon oil of low hydrogen content and polyethers to react under chain-transfer agent, catalyst action, introducing contains amino coupling agent and contains the epoxy group(ing) coupling agent again, prepares amino/epoxy co-modified hydrophilic silicon oil.Fabric after the arrangement has extremely low surface tension, and existing good flexibility can be returned something for repairs not yellowing again.Prepared a kind of hydrophilic amino silicone oil among the patent CN1631892A, cardinal principle is: the amino coupling agent that adopt low viscous hydroxy silicon oil and cyclosiloxane, contains the polyethers chain link is a raw material, adopting alcohol or ester is solvent, make it in solvent, carry out condensation reaction, just can make hydrophilic amino silicone oil.The amido silicon oil of gained need not can directly be scattered in the water in emulsification, breakdown of emulsion or floating oil phenomenon can not occur in the process of using, and more can not form oil mark on lining, and lining after treatment still can keep good hydrophilicity in addition.
Polyether modified epoxy/amido silicon oil of the present invention is to introduce polyether segment on the polysiloxane macromolecular chain, epoxy group(ing) and amino silicone oil, its preparation method is to adopt hydrogen-containing amino silicone oil, thiazolinyl epoxy compounds, active polyether to react under the platinum catalyst effect, prepares polyether modified epoxy/amido silicon oil.
Summary of the invention
The objective of the invention is to overcome above-mentioned weak point, can directly carry out modification to amido silicon oil thereby provide a kind of, reactions steps is simple, reaction conditions is gentle simple; Fabric through putting in order had out both kept soft, the smooth fine quality of common amido silicon oil, and the while is the good characteristics of possess hydrophilic property again; In use be difficult for floating oil, can reduce yellowing, and can strengthen the preparation method of a kind of polyether modified epoxy/amido silicon oil of washing fastness.
According to technical scheme provided by the invention, a kind of preparation method of polyether modified epoxy/amido silicon oil adopts following processing step: its formula rate is counted by weight:
Hydrogen-containing amino silicone oil 40-50 part, thiazolinyl epoxy compounds 20-30 part, active polyether 2.5-3 part, Virahol 20-30 part are added in the reactor, logical nitrogen stirred 0.8～1.2 hour, be warming up to 90-95 ℃, in 0.5～1.2 hour, drip off catalyzer 0.5-2 part, reacted 4～6 hours, remove Virahol with vacuumizing then, promptly obtain polyether modified epoxy/amido silicon oil product.
The described vacuum tightness that vacuumizes :-20KPa.
Described nitrogen flow: 16m
3/ hour.
Described active polyether is allyl polyether or allyl alcohol polyether or vinylcarbinol polyethers.
Described catalyzer is a liquid platinum.
Described thiazolinyl epoxy compounds thiazolinyl epoxy butanols or thiazolinyl butylene oxide ring or thiazolinyl R-GLYCIDOL.
Polyether modified epoxy/amido silicon oil of the present invention can be used for the softening of fabric, and step is as follows:
1, cotton fabrics two is soaked two and roll, pressure is 2～5kg/cm
2, pick-up is 60%～75%;
2, dry 2～5min down at 70～100 ℃;
3, under 150～180 ℃, bake 15～30s again.
Compared with the prior art the present invention has the following advantages:
1, the present invention directly carries out modification to amido silicon oil, and reactions steps is simple, reaction conditions is gentle simple.
2, the fabric put in order out of polyether modified epoxy/amido silicon oil had both kept soft, the smooth fine quality of common amido silicon oil, simultaneously good characteristics of possess hydrophilic property again.
3, be difficult for floating oil in storage and the use, reduced yellowing, strengthened washing fastness, be particularly suitable for the arrangement of light fabric.
4, bake the processing fabric by padding, technology is simple, and process does not have hazardous solvent volatilization, safety and environmental protection.
Embodiment
Following the present invention will be further described in conjunction with the embodiments:
Embodiment 1: the preparation method of a kind of polyether modified epoxy/amido silicon oil of the present invention adopts following processing step: its formula rate is counted by weight:
1, the preparation of polyether modified epoxy/amido silicon oil
50 parts of hydrogen-containing amino silicone oil, 25 parts of thiazolinyl epoxidation butanols, 2.5 parts of allyl polyethers, 22 parts of Virahols are added in the reactor, and logical nitrogen is with 16m
3/ hour flow stirred 1 hour, be warming up to 90 ℃, in 1 hour, drip off 0.5 part of liquid platinum, reacted 5 hours, then with vacuumize remove Virahol (vacuum tightness :-20Kpa), obtain viscous liquid and be polyether modified epoxy/amido silicon oil product.Detected result viscosity: 4250mpas.
2, the preparation of polyether modified epoxy/amino silicon oil emulsion:
In the there-necked flask of the 1000ml that agitator is housed, add 800g soft water, start polyether modified epoxy/amido silicon oil 200g that agitator slowly adds method for preparing, added in about 10 minutes, can obtain content and be polyether modified epoxy/amino silicon oil emulsion of 20%.
3, textile finishing and performance test
It is 20% emulsion that the polyether modified epoxy/amido silicon oil that makes is made into content, and other gets common amido silicon oil, and to be made into amido silicon oil water content reason be 20% solution.Bath raio 1: 20 is soaked two roll process by two cotton fabric is carried out softening, and (40tex * 40tex) two soaks two and rolls in polyether modified epoxy/amino silicon oil emulsion cotton fabrics, and pressure is 3kg/cm
2, pick-up is 75%, dries 5min down for 100 ℃ in convection oven, bakes 30s under 160 ℃.Measure the whiteness of fabric with the WSB-2 blancometer; Please at least five people are blind touches for feel, evaluation rank (wherein 6 grades best, 1 grade the poorest); Wetting ability adopts the water droplet osmose process to measure.
Table 1 embodiment 1 The performance test results
| Blank | Common amido silicon oil | Embodiment | |
| Feel | The 1-2 level | The 5-6 level | The 5-6 level |
| Whiteness | 54.6 | 46.1 | 50.5 |
| Wetting ability | 0.92 | 225.09 | 30.24 |
Embodiment 2: the preparation method of a kind of polyether modified epoxy/amido silicon oil of the present invention adopts following processing step: its formula rate is counted by weight:
1, the preparation of polyether modified epoxy/amido silicon oil
45 parts of hydrogen-containing amino silicone oil, 22 parts of thiazolinyl butylene oxide rings, 3 parts of allyl alcohol polyethers, 29 parts of Virahols are added in the reactor, and logical nitrogen is with 16m
3/ hour flow stirred 0.8 hour, be warming up to 93 ℃, in 0.8 hour, drip off 1 part of liquid platinum, reacted 4 hours, then with vacuumize remove Virahol (vacuum tightness :-20Kpa), obtain viscous liquid and be polyether modified epoxy/amido silicon oil product.Detected result viscosity: 4150mpas.
2, the preparation of polyether modified epoxy/amino silicon oil emulsion:
In the there-necked flask of the 1000ml that agitator is housed, add 800g soft water, start polyether modified epoxy/amido silicon oil 200g that agitator slowly adds method for preparing, added in about 10 minutes, can obtain content and be polyether modified epoxy/amino silicon oil emulsion of 20%.
3, textile finishing
Wash/cotton mixed machine fabric two soaks two and rolls in silicone oil emulsion, and pressure is 4kg/cm
2, pick-up is 75%, dries 4min down for 100 ℃ in convection oven, bakes 15s under 160 ℃.
4, performance test
Table 2 embodiment 2 The performance test results
| Blank | Common amido silicon oil | Embodiment | |
| Feel | The 1-2 level | The 5-6 level | 5 grades |
| Whiteness | 54.6 | 46.1 | 52.4 |
| Wetting ability | 0.92 | 225.09 | 26.32 |
Embodiment 3: the preparation method of a kind of polyether modified epoxy/amido silicon oil of the present invention adopts following processing step: its formula rate is counted by weight:
1, the preparation of polyether modified epoxy/amido silicon oil
45 parts of hydrogen-containing amino silicone oil, 28 parts of thiazolinyl R-GLYCIDOLs, 3 parts of vinylcarbinol polyethers, 23 parts of Virahols are added in the reactor, and logical nitrogen is with 16m
3/ hour flow stirred 1.2 hours, be warming up to 95 ℃, in 1.2 hours, drip off 1 part of liquid platinum, reacted 6 hours, then with vacuumize remove Virahol (vacuum tightness :-20Kpa), obtain viscous liquid and be polyether modified epoxy/amido silicon oil product.Detected result viscosity: 4200mpas.
2, the preparation of polyether modified epoxy/amino silicon oil emulsion:
In the there-necked flask of the 1000ml that agitator is housed, add 800g soft water, start polyether modified epoxy/amido silicon oil 200g that agitator slowly adds method for preparing, added in about 10 minutes, can obtain content and be polyether modified epoxy/amino silicon oil emulsion of 20%.
3, textile finishing
Wash/cotton mixed machine fabric two soaks two and rolls in silicone oil emulsion, and pressure is 3kg/cm
2, pick-up is 70%, dries 3min down for 90 ℃ in convection oven, bakes 20s under 150 ℃.
4, performance test
Table 2 embodiment 2 The performance test results
| Blank | Common amido silicon oil | Embodiment | |
| Feel | The 1-2 level | The 5-6 level | The 5-6 level |
| Whiteness | 54.6 | 46.1 | 48.7.4 |
| Wetting ability | 0.92 | 225.09 | 28.79 |
Claims (5)
1, a kind of preparation method of polyether modified epoxy/amido silicon oil is characterized in that adopting following processing step: its formula rate is counted by weight:
Hydrogen-containing amino silicone oil 40-50 part, thiazolinyl epoxy compounds 20-30 part, active polyether 2.5-3 part, Virahol 20-30 part are added in the reactor, logical nitrogen stirred 0.8～1.2 hour, be warming up to 90-95 ℃, in 0.5～1.2 hour, drip off catalyzer 0.5-2 part, reacted 4～6 hours, vacuumize then, remove Virahol, get product.
2, the preparation method of a kind of polyether modified epoxy/amido silicon oil according to claim 1 is characterized in that the described vacuum tightness that vacuumizes :-20Kpa.
3, the preparation method of a kind of polyether modified epoxy/amido silicon oil according to claim 1 is characterized in that described active polyether is allyl polyether or allyl alcohol polyether or vinylcarbinol polyethers.
4, the preparation method of a kind of polyether modified epoxy/amido silicon oil according to claim 1 is characterized in that described catalyzer is a liquid platinum.
5, the preparation method of a kind of polyether modified epoxy/amido silicon oil according to claim 1 is characterized in that described thiazolinyl epoxy compounds is thiazolinyl epoxy butanols or thiazolinyl butylene oxide ring or thiazolinyl R-GLYCIDOL.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910029295A CN101525438A (en) | 2009-04-08 | 2009-04-08 | Method for preparing polyether modified epoxy/amino silicone oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910029295A CN101525438A (en) | 2009-04-08 | 2009-04-08 | Method for preparing polyether modified epoxy/amino silicone oil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101525438A true CN101525438A (en) | 2009-09-09 |
Family
ID=41093520
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910029295A Pending CN101525438A (en) | 2009-04-08 | 2009-04-08 | Method for preparing polyether modified epoxy/amino silicone oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101525438A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102675652A (en) * | 2012-05-18 | 2012-09-19 | 陕西科技大学 | Preparation method of crosslinking-modified pectinate polyether amino-silicone oil |
| CN103193984A (en) * | 2012-01-04 | 2013-07-10 | 安徽科光新材料有限公司 | Hydrophilic aminosilicon oil, and preparation method and uses thereof |
| CN103193981A (en) * | 2012-01-04 | 2013-07-10 | 安徽科光新材料有限公司 | Hydrophilic aminosilicon oil, and preparation method and uses thereof |
| CN103193982A (en) * | 2012-01-04 | 2013-07-10 | 安徽科光新材料有限公司 | Hydrophilic organic silicon silk fabric finishing agent, and preparation method and uses thereof |
| CN104452311A (en) * | 2014-11-25 | 2015-03-25 | 浙江传化股份有限公司 | Method for preparing side-chain-modified organosilicon softener |
| CN105111450A (en) * | 2015-09-24 | 2015-12-02 | 天津市利顺达粘合剂有限公司 | Synthesis method of water-soluble silicone oil used for treating leather |
| CN107938353A (en) * | 2017-11-30 | 2018-04-20 | 英泰时尚服饰（苏州）有限公司 | A kind of acrylic fabric and its soft fire-retardant composite finishing method |
| CN109503847A (en) * | 2018-11-15 | 2019-03-22 | 纳派化学(上海)有限公司 | A kind of preparation method of antistatic silicone oil |
| CN109535366A (en) * | 2018-11-16 | 2019-03-29 | 上海东大化学有限公司 | A kind of secondary amino silanes modified polyether polymer and preparation method thereof |
| CN114133573A (en) * | 2021-10-27 | 2022-03-04 | 浙江汉邦新材料股份有限公司 | Environment-friendly odorless hydrophilic organic silicon softening agent for wool tops and preparation method thereof |
-
2009
- 2009-04-08 CN CN200910029295A patent/CN101525438A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103193982B (en) * | 2012-01-04 | 2015-09-02 | 安徽科光新材料有限公司 | A kind of hydrophilic organosilicon silk fabric fabric finishing agent and its production and use |
| CN103193984A (en) * | 2012-01-04 | 2013-07-10 | 安徽科光新材料有限公司 | Hydrophilic aminosilicon oil, and preparation method and uses thereof |
| CN103193981A (en) * | 2012-01-04 | 2013-07-10 | 安徽科光新材料有限公司 | Hydrophilic aminosilicon oil, and preparation method and uses thereof |
| CN103193982A (en) * | 2012-01-04 | 2013-07-10 | 安徽科光新材料有限公司 | Hydrophilic organic silicon silk fabric finishing agent, and preparation method and uses thereof |
| CN103193981B (en) * | 2012-01-04 | 2016-08-03 | 安徽科光新材料有限公司 | A kind of hydrophilic amido silicon oil and its production and use |
| CN102675652B (en) * | 2012-05-18 | 2014-04-16 | 陕西科技大学 | Preparation method of crosslinking-modified pectinate polyether amino-silicone oil |
| CN102675652A (en) * | 2012-05-18 | 2012-09-19 | 陕西科技大学 | Preparation method of crosslinking-modified pectinate polyether amino-silicone oil |
| CN104452311A (en) * | 2014-11-25 | 2015-03-25 | 浙江传化股份有限公司 | Method for preparing side-chain-modified organosilicon softener |
| CN104452311B (en) * | 2014-11-25 | 2017-02-22 | 杭州传化精细化工有限公司 | Method for preparing side-chain-modified organosilicon softener |
| CN105111450A (en) * | 2015-09-24 | 2015-12-02 | 天津市利顺达粘合剂有限公司 | Synthesis method of water-soluble silicone oil used for treating leather |
| CN107938353A (en) * | 2017-11-30 | 2018-04-20 | 英泰时尚服饰（苏州）有限公司 | A kind of acrylic fabric and its soft fire-retardant composite finishing method |
| CN109503847A (en) * | 2018-11-15 | 2019-03-22 | 纳派化学(上海)有限公司 | A kind of preparation method of antistatic silicone oil |
| CN109535366A (en) * | 2018-11-16 | 2019-03-29 | 上海东大化学有限公司 | A kind of secondary amino silanes modified polyether polymer and preparation method thereof |
| CN114133573A (en) * | 2021-10-27 | 2022-03-04 | 浙江汉邦新材料股份有限公司 | Environment-friendly odorless hydrophilic organic silicon softening agent for wool tops and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101525438A (en) | Method for preparing polyether modified epoxy/amino silicone oil | |
| CN102644200B (en) | Super-soft finishing agent of silicone oil | |
| CN102643435A (en) | Supersoft hydrophilic block silicone oil compound and preparation method thereof | |
| CN101418518A (en) | Method for preparing durable hydrophilic polyether modified amino polysiloxane soft agent | |
| CN105155280A (en) | Ice feeling finishing agent and preparation method thereof | |
| CN106589385A (en) | Low-yellowing quaternary ammonium type hydrophilic amino-modified silicone oil emulsion and preparation method thereof | |
| CN102634036B (en) | Novel linear amino and polyester modified organosilicon compound for textiles | |
| CN105755837B (en) | A kind of preparation method of quaternised modified amino-silicone oil softener and application | |
| CN111303342B (en) | Dust remover for cotton knitted fabric and preparation method thereof | |
| CN102660029B (en) | Cation modified supersoft hydrophilic block silicone oil compound and preparation method and application | |
| CN111410751A (en) | Preparation method of amphoteric organic silicon polymer emulsion | |
| CN102643436B (en) | Supersoft hydrophilic block silicone oil intermediate compound and preparation method thereof | |
| CN108486899B (en) | Fabric softening finishing agent and preparation method thereof | |
| CN102585229B (en) | Polyether/aminopolysiloxane block copolymer and use thereof | |
| CN112726211A (en) | Preparation method of polyurethane modified organic silicon softening agent | |
| EP3253915B1 (en) | Alkoxylated polyethyleneimine hydrophilically-modified fibers | |
| CN103132330A (en) | Textile having shape memory interpenetrating polymer network | |
| CN112900103A (en) | Antibacterial soft composition and preparation method thereof | |
| CN110312830A (en) | Alkoxylate polyethyleneimine and composition containing it | |
| CN107475861A (en) | A kind of preparation method of the stretch-proof fabric containing chitosan | |
| CN101338520A (en) | Organosilicon composite multifunction spinning dressing agent | |
| CN111155317A (en) | Chlorine-resistant hydrophilic softening agent and preparation method and application thereof | |
| CN114106337B (en) | Ternary polymerization hydrophilic amino silicone oil, preparation method thereof and finishing agent | |
| CN108951169B (en) | Preparation method of natural alcohol ether modified organosilicon hydrophilic softening agent | |
| CN106947083B (en) | Preparation method and application of organic silicon antistatic agent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20090909 |