CN104592527A - Preparation method of modified silicone oil surfactant for textile - Google Patents
Preparation method of modified silicone oil surfactant for textile Download PDFInfo
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- CN104592527A CN104592527A CN201510068538.0A CN201510068538A CN104592527A CN 104592527 A CN104592527 A CN 104592527A CN 201510068538 A CN201510068538 A CN 201510068538A CN 104592527 A CN104592527 A CN 104592527A
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Abstract
The invention discloses a preparation method of a modified silicone oil surfactant for textile. The preparation method comprises the following steps: preparing hydrogen-containing silicone oil; preparing methyl methacrylate modified silicone oil; and preparing a polyether amide modified silicone oil surfactant to finally obtain the modified silicone oil surfactant. The preparation method provided by the invention is simple in process steps, easy to control, small in injury to a human body in an operation process, small in pollution, energy-saving, emission-reducing and short in reaction time; the prepared surfactant is good in stability, good in hydrophilcity, easier to self-emulsify and better in emulsion stability, and has the characteristics of low surface tension and high activity.
Description
Technical field
The invention belongs to textile auxiliary agent field, be specifically related to a kind of weaving by the preparation method of modified silicon oil tensio-active agent.
Background technology
In weaving garment industry, organic silicon surfactant is a kind of important auxiliary agent, this is because its raw materials cost is low on the one hand, asepsis environment-protecting, it can be used for the aftertreatment of fabric as softening agent, water-resisting agent, anti-melting finishing composition, static inhibitor, sanitary finish agent, lubricant, defoamer and shrinkproof wrinkle agent on the other hand, can improve elasticity, make fabric have slipping, resistance to crapyness, static resistance, moisture absorption water vapour permeability and soil release performance.
In recent years, the requirement that fast development and people along with science and technology apply organic silicon surfactant is more and more higher, and the organic silicon surfactant of simple function is difficult to practical requirement.In this case, develop multi-functional organic silicon surfactant, modification is again carried out to modified silicon oil, give the important directions that its more more outstanding performance becomes organosilicon material development.Wherein in fabric treating, organic silicon surfactant is a kind of important textile finishing auxiliary agent.By to some fabrics, as cotton, fur, burlap arrange, their feel can be solved coarse, the shortcoming such as ventilative not.
On textile finishing, common quaternary ammonium salt surfactivity antiseptic-germicide belongs to dissolution type, very not washable, and easily lost efficacy and be enriched in human body surface, life-time service is harmful.But quaternary ammonium salt organosilicon cationic tensio-active agent and fiber are in conjunction with for a long time fastening, antibacterial effect is remarkable, belong to non-dissolving type antibacterial finishing agent, to human non-toxic's safety, there is good inhibition to Gram-negative bacteria, yeast and fungi etc., be therefore widely used in the arrangement of towel, carpet, socks, sheet, underwear and operation textile; The features such as Nonionic organosilicon surfactant has high surface, dispersing property is excellent, consumption is few, defoaming capacity is strong and action effect is lasting, are mainly applied in textile industry as defoamer and hydrophilic finishing agent.
Summary of the invention
Technical problem to be solved by this invention is, for the shortcoming that above prior art exists, proposes a kind of weaving and uses the preparation method of modified silicon oil tensio-active agent, this preparation method's processing step is simple, be easy to control, little to the injury of human body in operating process, pollute little, energy-saving and emission-reduction, reaction times is short, and the surfactant stability prepared is good, good hydrophilic property, self-emulsifying is easier and stability of emulsion is better, has low surface tension, highly active feature simultaneously.
The technical scheme that the present invention solves above technical problem is:
Weave by a preparation method for modified silicon oil tensio-active agent, specifically comprise the following steps:
(1) preparation of containing hydrogen silicone oil
(1) soak Zeo-karb 24h with concentrated hydrochloric acid, then use deionized water rinsing 3-5 time, then soak Zeo-karb 24h with deionized water, finally take out Zeo-karb and dry stand-by in the vacuum drying oven of 85 DEG C;
(2) under agitation, 2 are added successively in there-necked flask, 4, 6, 8-tetramethyl-ring tetrasiloxane, octamethylcyclotetrasiloxane, hexamethyldisiloxane and catalyst cation exchange resin after treatment, be heated to 80 DEG C and start stirring reaction, stop after reaction 6-8h stirring and heating, catalyst cation exchange resin is leached with 200 object filter screens after cooling, subsequently filtrate decompression is distilled, remove low boilers, obtain containing hydrogen silicone oil, wherein 2, 4, 6, 8-tetramethyl cyclotetrasiloxane: octamethylcyclotetrasiloxane: hexamethyldisiloxane mass ratio is: 20-25:10-15:0.8-1, catalyst cation exchange resin consumption is the 5-6% of 2,4,6,8-tetramethyl cyclotetrasiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane total mass,
(2) preparation of methyl methacrylate-modified silicone oil
(1) add in the there-necked flask that reflux condensing tube is housed obtained containing hydrogen silicone oil, methyl methacrylate, toluene and massfraction be 0.5% isopropyl alcohol solution of chloroplatinic acid mix, wherein containing hydrogen silicone oil: methyl methacrylate: the mass ratio of toluene is 20-25:22-28:10-13; The consumption of isopropyl alcohol solution of chloroplatinic acid is the 0.005-0.008% of containing hydrogen silicone oil, methyl methacrylate and toluene total amount;
(2) install reaction unit, start heated and stirred, after 85 DEG C after isothermal reaction 10h, stopped reaction;
(3) toluene and remaining methyl methacrylate are gone out in underpressure distillation, and residuum is dissolved in ethanol, centrifugation, isolates precipitation, and distillation removing ethanol, obtains water white product;
(3) preparation of polyetheramides modified silicon oil tensio-active agent
(1) in the there-necked flask that reflux condensing tube is housed, obtained methyl methacrylate-modified silicone oil, polyetheramine ED2003, toluene and catalyzer aluminum chloride is added; Wherein methyl methacrylate-modified silicone oil: polyetheramine ED2003: the mass ratio of toluene is: 20-25:2-5:6-10; Catalyzer aluminum chloride consumption is the 0.004-0.005% of methyl methacrylate-modified silicone oil, polyetheramine ED2003 and toluene total amount;
(2) install fractionation plant, reflux at 80 DEG C, stir, fractionate out methyl alcohol, until after the amount of the methyl alcohol fractionated out no longer changes, stopped reaction;
(3) underpressure distillation removing solvent toluene, Filtration of catalyst aluminum chloride and remaining polyetheramine, obtain pale yellow transparent product and modified silicon oil tensio-active agent.
The technical scheme that the present invention limits further is:
In the preparation method of aforementioned weaving modified silicon oil tensio-active agent, catalyst cation exchange resin is NKC-9 Zeo-karb.
In the preparation method of aforementioned weaving modified silicon oil tensio-active agent, catalyst particle size is 0.4-0.6mm, and hydrogen ion molality is 6-8mmol/g.
The invention has the beneficial effects as follows: the silicone oil of this amino by polyetheramine of (1) the present invention and band functional group carries out aminolysis reaction and obtains polyetheramides modified silicon oil, give full play to amino modified and polyether-modified two-fold advantage, polyether segment is linked on silicone molecule, improve molecular hydrophylic, emulsification can be carried out without the need to additional emulsifying agent, good emulsion stability, there will not be problems such as " breakdown of emulsion floating oils ".(2) in modifying process of the present invention, primary amino has become secondary amino group after the reaction, and stability is better, and xanthochromia is lower, improves the performance of organosilicon auxiliary agent further.(3) domesticly at present in the synthesis of modified silicon oil, traditional concentrated sulfuric acid catalyst is still adopted, such catalyzer can affect the quality of product, cause silicone oil product ubiquity unstable, trace impurity is many, the shortcomings such as batch wise differences is large, and the strong-acid cation-exchange resin catalyst adopted in the present invention can solve silicone oil product department stable problem, and it is easy to control to synthesis silicone oil reaction process, stable operation, little to human injury, Reaction time shorten, can reclaim and reuse repeatedly, energy-saving and emission-reduction, the advantages such as decreasing pollution.(4) in the present invention, synthesizing methylmethacrylate modified silicon oil adopts containing hydrogen silicone oil and methyl methacrylate to carry out addition reaction to obtain, and step is simple, and be easy to control, the product stability of generation is good.(5) a kind of polyetheramides modified silicon oil of the present invention is a kind of novel organosilicon nonionogenic tenside, wherein siloxanes segment has lipophilicity, polyether segment, amino have wetting ability, better than the wetting ability of general amino-modified silicone oil, self-emulsifying more easily and stability of emulsion more, there is the intrinsic low surface tension of polysiloxane, highly active feature simultaneously.
Embodiment
embodiment 1
The present embodiment provides a kind of and weaves by the preparation method of modified silicon oil tensio-active agent, specifically comprises the following steps:
(1) preparation of containing hydrogen silicone oil
(1) soaking particle diameter with concentrated hydrochloric acid is 0.4mm, hydrogen ion molality is the NKC-9 Zeo-karb 24h of 7mmol/g, then deionized water rinsing is used 3 times, then soak NKC-9 Zeo-karb 24h with deionized water, finally take out NKC-9 Zeo-karb and dry stand-by in the vacuum drying oven of 85 DEG C;
(2) under agitation, 2 are added successively in there-necked flask, 4, 6, 8-tetramethyl-ring tetrasiloxane, octamethylcyclotetrasiloxane, hexamethyldisiloxane and catalyst n KC-9 Zeo-karb after treatment, be heated to 80 DEG C and start stirring reaction, stop after reaction 6h stirring and heating, catalyst n KC-9 Zeo-karb is leached with 200 object filter screens after cooling, subsequently filtrate decompression is distilled, remove low boilers, obtain containing hydrogen silicone oil, wherein 2, 4, 6, 8-tetramethyl cyclotetrasiloxane: octamethylcyclotetrasiloxane: hexamethyldisiloxane mass ratio is 20:12:0.8, catalyst n KC-9 Zeo-karb consumption is 6% of 2,4,6,8-tetramethyl cyclotetrasiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane total mass,
(2) preparation of methyl methacrylate-modified silicone oil
(1) add in the there-necked flask that reflux condensing tube is housed obtained containing hydrogen silicone oil, methyl methacrylate, toluene and massfraction be 0.5% isopropyl alcohol solution of chloroplatinic acid mix, wherein containing hydrogen silicone oil: methyl methacrylate: the mass ratio of toluene is 25:25:12; The consumption of isopropyl alcohol solution of chloroplatinic acid is 0.006% of containing hydrogen silicone oil, methyl methacrylate and toluene total amount;
(2) install reaction unit, start heated and stirred, after 85 DEG C after isothermal reaction 10h, stopped reaction;
(3) toluene and remaining methyl methacrylate are gone out in underpressure distillation, and residuum is dissolved in ethanol, centrifugation, isolates precipitation, and distillation removing ethanol, obtains water white product;
(3) preparation of polyetheramides modified silicon oil tensio-active agent
(1) in the there-necked flask that reflux condensing tube is housed, obtained methyl methacrylate-modified silicone oil, polyetheramine ED2003, toluene and catalyzer aluminum chloride is added; Wherein methyl methacrylate-modified silicone oil: polyetheramine ED2003: the mass ratio of toluene is 25:4:8; Catalyzer aluminum chloride consumption is 0.004% of methyl methacrylate-modified silicone oil, polyetheramine ED2003 and toluene total amount;
(2) install fractionation plant, reflux at 80 DEG C, stir, fractionate out methyl alcohol, until after the amount of the methyl alcohol fractionated out no longer changes, stopped reaction;
(3) underpressure distillation removing solvent toluene, Filtration of catalyst aluminum chloride and remaining polyetheramine, obtain pale yellow transparent product and modified silicon oil tensio-active agent.
embodiment 2
The present embodiment provides a kind of and weaves by the preparation method of modified silicon oil tensio-active agent, specifically comprises the following steps:
(1) preparation of containing hydrogen silicone oil
(1) soaking particle diameter with concentrated hydrochloric acid is 0.5mm, hydrogen ion molality is the NKC-9 Zeo-karb 24h of 8mmol/g, then deionized water rinsing is used 4 times, then soak NKC-9 Zeo-karb 24h with deionized water, finally take out NKC-9 Zeo-karb and dry stand-by in the vacuum drying oven of 85 DEG C;
(2) under agitation, 2 are added successively in there-necked flask, 4, 6, 8-tetramethyl-ring tetrasiloxane, octamethylcyclotetrasiloxane, hexamethyldisiloxane and catalyst n KC-9 Zeo-karb after treatment, be heated to 80 DEG C and start stirring reaction, stop after reaction 8h stirring and heating, catalyst n KC-9 Zeo-karb is leached with 200 object filter screens after cooling, subsequently filtrate decompression is distilled, remove low boilers, obtain containing hydrogen silicone oil, wherein 2, 4, 6, 8-tetramethyl cyclotetrasiloxane: octamethylcyclotetrasiloxane: hexamethyldisiloxane mass ratio is 25:10:1, catalyst n KC-9 Zeo-karb consumption is 5% of 2,4,6,8-tetramethyl cyclotetrasiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane total mass,
(2) preparation of methyl methacrylate-modified silicone oil
(1) add in the there-necked flask that reflux condensing tube is housed obtained containing hydrogen silicone oil, methyl methacrylate, toluene and massfraction be 0.5% isopropyl alcohol solution of chloroplatinic acid mix, wherein containing hydrogen silicone oil: methyl methacrylate: the mass ratio of toluene is 22:28:10; The consumption of isopropyl alcohol solution of chloroplatinic acid is 0.005% of containing hydrogen silicone oil, methyl methacrylate and toluene total amount;
(2) install reaction unit, start heated and stirred, after 85 DEG C after isothermal reaction 10h, stopped reaction;
(3) toluene and remaining methyl methacrylate are gone out in underpressure distillation, and residuum is dissolved in ethanol, centrifugation, isolates precipitation, and distillation removing ethanol, obtains water white product;
(3) preparation of polyetheramides modified silicon oil tensio-active agent
(1) in the there-necked flask that reflux condensing tube is housed, obtained methyl methacrylate-modified silicone oil, polyetheramine ED2003, toluene and catalyzer aluminum chloride is added; Wherein methyl methacrylate-modified silicone oil: polyetheramine ED2003: the mass ratio of toluene is 20:5:6; Catalyzer aluminum chloride consumption is 0.005% of methyl methacrylate-modified silicone oil, polyetheramine ED2003 and toluene total amount;
(2) install fractionation plant, reflux at 80 DEG C, stir, fractionate out methyl alcohol, until after the amount of the methyl alcohol fractionated out no longer changes, stopped reaction;
(3) underpressure distillation removing solvent toluene, Filtration of catalyst aluminum chloride and remaining polyetheramine, obtain pale yellow transparent product and modified silicon oil tensio-active agent.
embodiment 3
The present embodiment provides a kind of and weaves by the preparation method of modified silicon oil tensio-active agent, specifically comprises the following steps:
(1) preparation of containing hydrogen silicone oil
(1) soaking particle diameter with concentrated hydrochloric acid is 0.6mm, hydrogen ion molality is the NKC-9 Zeo-karb 24h of 6mmol/g, then deionized water rinsing is used 5 times, then soak NKC-9 Zeo-karb 24h with deionized water, finally take out NKC-9 Zeo-karb and dry stand-by in the vacuum drying oven of 85 DEG C;
(2) under agitation, 2 are added successively in there-necked flask, 4, 6, 8-tetramethyl-ring tetrasiloxane, octamethylcyclotetrasiloxane, hexamethyldisiloxane and catalyst n KC-9 Zeo-karb after treatment, be heated to 80 DEG C and start stirring reaction, stop after reaction 7h stirring and heating, catalyst n KC-9 Zeo-karb is leached with 200 object filter screens after cooling, subsequently filtrate decompression is distilled, remove low boilers, obtain containing hydrogen silicone oil, wherein 2, 4, 6, 8-tetramethyl cyclotetrasiloxane: octamethylcyclotetrasiloxane: hexamethyldisiloxane mass ratio is 22:15:0.9, catalyst n KC-9 Zeo-karb consumption is 5% of 2,4,6,8-tetramethyl cyclotetrasiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane total mass,
(2) preparation of methyl methacrylate-modified silicone oil
(1) add in the there-necked flask that reflux condensing tube is housed obtained containing hydrogen silicone oil, methyl methacrylate, toluene and massfraction be 0.5% isopropyl alcohol solution of chloroplatinic acid mix, wherein containing hydrogen silicone oil: methyl methacrylate: the mass ratio of toluene is 20:22:13; The consumption of isopropyl alcohol solution of chloroplatinic acid is 0.008% of containing hydrogen silicone oil, methyl methacrylate and toluene total amount;
(2) install reaction unit, start heated and stirred, after 85 DEG C after isothermal reaction 10h, stopped reaction;
(3) toluene and remaining methyl methacrylate are gone out in underpressure distillation, and residuum is dissolved in ethanol, centrifugation, isolates precipitation, and distillation removing ethanol, obtains water white product;
(3) preparation of polyetheramides modified silicon oil tensio-active agent
(1) in the there-necked flask that reflux condensing tube is housed, obtained methyl methacrylate-modified silicone oil, polyetheramine ED2003, toluene and catalyzer aluminum chloride is added; Wherein methyl methacrylate-modified silicone oil: polyetheramine ED2003: the mass ratio of toluene is 23:2:10; Catalyzer aluminum chloride consumption is 0.005% of methyl methacrylate-modified silicone oil, polyetheramine ED2003 and toluene total amount;
(2) install fractionation plant, reflux at 80 DEG C, stir, fractionate out methyl alcohol, until after the amount of the methyl alcohol fractionated out no longer changes, stopped reaction;
(3) underpressure distillation removing solvent toluene, Filtration of catalyst aluminum chloride and remaining polyetheramine, obtain pale yellow transparent product and modified silicon oil tensio-active agent.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of application claims.
Claims (3)
1. weave by a preparation method for modified silicon oil tensio-active agent, it is characterized in that, specifically comprise the following steps:
(1) preparation of containing hydrogen silicone oil
(1) soak Zeo-karb 24h with concentrated hydrochloric acid, then use deionized water rinsing 3-5 time, then soak Zeo-karb 24h with deionized water, finally take out Zeo-karb and dry stand-by in the vacuum drying oven of 85 DEG C;
(2) under agitation, 2 are added successively in there-necked flask, 4, 6, 8-tetramethyl-ring tetrasiloxane, octamethylcyclotetrasiloxane, hexamethyldisiloxane and catalyst cation exchange resin after treatment, be heated to 80 DEG C and start stirring reaction, stop after reaction 6-8h stirring and heating, catalyst cation exchange resin is leached with 200 object filter screens after cooling, subsequently filtrate decompression is distilled, remove low boilers, obtain containing hydrogen silicone oil, wherein 2, 4, 6, 8-tetramethyl cyclotetrasiloxane: octamethylcyclotetrasiloxane: hexamethyldisiloxane mass ratio is: 20-25:10-15:0.8-1, catalyst cation exchange resin consumption is the 5-6% of 2,4,6,8-tetramethyl cyclotetrasiloxane, octamethylcyclotetrasiloxane and hexamethyldisiloxane total mass,
(2) preparation of methyl methacrylate-modified silicone oil
(1) add in the there-necked flask that reflux condensing tube is housed obtained containing hydrogen silicone oil, methyl methacrylate, toluene and massfraction be 0.5% isopropyl alcohol solution of chloroplatinic acid mix, wherein containing hydrogen silicone oil: methyl methacrylate: the mass ratio of toluene is 20-25:22-28:10-13; The consumption of isopropyl alcohol solution of chloroplatinic acid is the 0.005-0.008% of containing hydrogen silicone oil, methyl methacrylate and toluene total amount;
(2) install reaction unit, start heated and stirred, after 85 DEG C after isothermal reaction 10h, stopped reaction;
(3) toluene and remaining methyl methacrylate are gone out in underpressure distillation, and residuum is dissolved in ethanol, centrifugation, isolates precipitation, and distillation removing ethanol, obtains water white product;
(3) preparation of polyetheramides modified silicon oil tensio-active agent
(1) in the there-necked flask that reflux condensing tube is housed, obtained methyl methacrylate-modified silicone oil, polyetheramine ED2003, toluene and catalyzer aluminum chloride is added; Wherein methyl methacrylate-modified silicone oil: polyetheramine ED2003: the mass ratio of toluene is: 20-25:2-5:6-10; Catalyzer aluminum chloride consumption is the 0.004-0.005% of methyl methacrylate-modified silicone oil, polyetheramine ED2003 and toluene total amount;
(2) install fractionation plant, reflux at 80 DEG C, stir, fractionate out methyl alcohol, until after the amount of the methyl alcohol fractionated out no longer changes, stopped reaction;
(3) underpressure distillation removing solvent toluene, Filtration of catalyst aluminum chloride and remaining polyetheramine, obtain pale yellow transparent product and modified silicon oil tensio-active agent.
2. weave by the preparation method of modified silicon oil tensio-active agent according to claim 1, it is characterized in that: described catalyst cation exchange resin is NKC-9 Zeo-karb.
3. weave according to claim 2 by the preparation method of modified silicon oil tensio-active agent, it is characterized in that: described catalyst particle size is 0.4-0.6mm, hydrogen ion molality is 6-8mmol/g.
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| CN109610004A (en) * | 2019-01-09 | 2019-04-12 | 上海交通大学 | A kind of method of modifying on calcium sulfate crystal whiskers surface |
| CN113274340A (en) * | 2021-06-23 | 2021-08-20 | 上海南滨江细胞生物科技有限公司 | Method for preparing moisturizing facial mask containing embryo extract |
| CN113563981A (en) * | 2021-07-06 | 2021-10-29 | 南京仁为医药科技有限公司 | Novel cationic organosilicon surfactant for multienzyme cleaning and preparation method thereof |
| CN113999688A (en) * | 2021-11-19 | 2022-02-01 | 西南石油大学 | Spreading agent for improving spreading performance of oil drop water surface |
| CN115160573A (en) * | 2022-07-15 | 2022-10-11 | 安徽信息工程学院 | Preparation method of hydrocarbon carboxyl modified silicone oil emulsion |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105220506A (en) * | 2015-11-03 | 2016-01-06 | 杭州传化精细化工有限公司 | A kind of block polyether eiastomeric silicone softener and its preparation method and application |
| CN105220506B (en) * | 2015-11-03 | 2018-01-19 | 杭州传化精细化工有限公司 | A kind of block polyether eiastomeric silicone softening agent and its preparation method and application |
| CN109610004A (en) * | 2019-01-09 | 2019-04-12 | 上海交通大学 | A kind of method of modifying on calcium sulfate crystal whiskers surface |
| CN113274340A (en) * | 2021-06-23 | 2021-08-20 | 上海南滨江细胞生物科技有限公司 | Method for preparing moisturizing facial mask containing embryo extract |
| CN113563981A (en) * | 2021-07-06 | 2021-10-29 | 南京仁为医药科技有限公司 | Novel cationic organosilicon surfactant for multienzyme cleaning and preparation method thereof |
| CN113563981B (en) * | 2021-07-06 | 2023-11-10 | 南京优洁境生物科技有限公司 | Novel cationic organosilicon surfactant for multienzyme cleaning and preparation method thereof |
| CN113999688A (en) * | 2021-11-19 | 2022-02-01 | 西南石油大学 | Spreading agent for improving spreading performance of oil drop water surface |
| CN115160573A (en) * | 2022-07-15 | 2022-10-11 | 安徽信息工程学院 | Preparation method of hydrocarbon carboxyl modified silicone oil emulsion |
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