CN103709326B - A kind of preparation method of cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent - Google Patents
A kind of preparation method of cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent Download PDFInfo
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- CN103709326B CN103709326B CN201310733427.8A CN201310733427A CN103709326B CN 103709326 B CN103709326 B CN 103709326B CN 201310733427 A CN201310733427 A CN 201310733427A CN 103709326 B CN103709326 B CN 103709326B
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Abstract
The present invention relates to laking agent technical field, a kind of cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent and preparation method thereof is provided, its key step is: adopt dimethyl diallyl ammonium chloride and organosilane monomer, sequestrant and deionized water mix, after logical nitrogen flooding oxygen, add initiator to carry out radical polymerization and can obtain cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent, the Final finishing that dyes is used for by adopting the obtained laking agent of method of the present invention, not only can improve the dry fastness to wet rubbing of anionic dyes dyeing, especially fastness to wet rubbing, and do not affect coloured light and keep fabrics feel soft, the laking agent utilizing preparation method of the present invention to obtain is not containing formaldehyde, nontoxic, environmental protection, it is a kind of novel dyeing and printing auxiliary.
Description
Technical field
The present invention relates to laking agent technical field, particularly cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent of one and preparation method thereof.
Background technology
Cotton fibre (main composition structure is Mierocrystalline cellulose) is as one of four large natural fibers (cotton, hair, silk, fiber crops), owing to certainly having the feel of good water absorbability, heat retention, comfortableness and softness in wear behavior aspect, and the feature such as cleaning and health care and degradable recycling is just more and more favored.In order to meet the demand of people to clothing fabric different colours, thus to dye to fabric.Dyestuff for cotton fiber dyeing has substantive dyestuff, matching stain and reactive dyestuffs etc. usually, and substantive dyestuff, matching stain and reactive dyestuffs are all anionic dyestuffs, all contain the water soluble group such as sulfonic group, carboxyl in molecule.Substantive dyestuff and matching stain all mainly anchor on fiber by Van der Waals force and hydrogen bond, and the fastness of set is limited, is easy to hydrolysis and fades in water, so generally all need the dyefastness improving fabric with laking agent.Containing reactive group in reactive dyestuff molecule structure, covalent linkage can be generated with fiber-reactive, so dyefastness is relatively high.But reactive dyestuffs are in dyeing course, and dyestuff unreacted reactant and hydrolyzate can not be completely clean, and this part dyestuff will fade, meanwhile, the covalent linkage contaminated on thing also can be hydrolyzed scission of link.Along with the raising that textile dyeing fastness requires, laking agent is also still needed to carry out fixation when contaminating some dark heavy colour fabrics.
Poly Dimethyl Diallyl Ammonium Chloride laking agent is as the ideal quaternary ammonium salt Polycationic aldehyde-free colour stabilizer of a class, it is obtained by radical polymerization with monomer diallyldimethylammonChloride Chloride, there is the structure such as five-ring, six-ring, be mainly five-membered ring structure.Its dye fixative theory is combined with ionic linkage with the negatively charged ion in dye structure by the quaternary ammonium salt cationic in structure and forms color lake to reach fixation object, simultaneously may have intermolecular forces effect comparatively closely due to its molecular chain modular construction and the similar feature of cotton fibre cellulosic structure, thus it should have good fixing property on cotton fibre, can be applicable on cotton fibre direct, the fixation of the dyestuffs such as sulfuration and activity, but because of itself and dyestuff ionic linkage effect and and cotton-textile fibres between van der Waals interaction be easily damaged under the effect of external force such as rubbing, especially fastness to wet rubbing is still not ideal enough to cause crock fastness.
Therefore modification is carried out to improve its every color fixation fastness, particularly fastness to wet rubbing to Poly Dimethyl Diallyl Ammonium Chloride structure, be still one of the focus and a difficult problem of research at present.
Summary of the invention
Therefore, for above content, the invention provides a kind of cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent and preparation method thereof, utilize the obtained laking agent of the method to be applied to fabric printing fixation last handling process, effectively can improve fabric and do wet friction colour fastness.
For achieving the above object, the present invention is achieved by the following technical solutions: a kind of preparation method of cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent, comprises the steps:
(1) by percentage to the quality, first sequestrant and the deionized water of 0.02 ~ 0.2 weight part is added in a kettle., be mixed with the chelating agent solution that mass percent concentration is 5% ~ 35%, stir after dissolving completely, add the dimethyl diallyl ammonium chloride of 35 ~ 49 weight parts and the organosilane monomer of 0.5 ~ 12 weight part again, mixing and stirring obtains mixing solutions;
(2) secondly, in reactor, lead to nitrogen 10 ~ 60 minutes with the speed of 50mL/min ~ 200mL/min, and start heat temperature raising;
(3) when temperature rises to 60 ~ 80 DEG C, then drip the initiator solution that mass percent concentration is 0.05 ~ 0.2 weight part of 1 ~ 10%, time for adding controls at 0.5 ~ 2 hour;
(4) polyreaction is carried out after dropwising, controlling the reaction times is 2 ~ 5 hours, finally add deionized water according to product requirement to carry out being diluted to setting concentration, after stirring, namely obtain cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent.
Further improvement is: in described step (1) sequestrant be in tripoly phosphate sodium STPP, Sodium hexametaphosphate 99, Trisodium Citrate, sodium tartrate, Sunmorl N 60S, disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate, nitrilotriacetic acid sodium, cyclohexanediaminetetraacetic acid sodium, diethylene triamine pentacetic acid (DTPA) sodium any one or two or more with arbitrarily than the mixture of mixing.
Further improvement is: the aqueous solution of dimethyl diallyl ammonium chloride to be mass percent concentration be 60 ± 0.5% or 65 ± 0.5% in described step (1).
Further improvement is: in described step (1), organosilane monomer is vinyltrimethoxy silane, vinyltriethoxysilane, vinyltriacetoxy silane, vinyl three ('beta '-methoxy oxyethyl group) silane, methacryloxypropyl trimethoxy silane, tetramethyl divinyl disiloxane, t etram-ethyltetravinylcyclotetrasiloxane or vinyl tributyl ketoximyl silane.
Further improvement is: the nitrogen in described step (2) is liquid nitrogen or the nitrogen of gaseous state.
Further improvement is: in described step (3) initiator be in ammonium persulphate, Sodium Persulfate and Potassium Persulphate any one or two or more with arbitrarily than the mixture of mixing.
The cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent adopting method of the present invention to prepare has higher positive charge density, ionic linkage can be combined into the negative charge of cellulose fiber peacekeeping dyestuff, the siloxane structure simultaneously introduced, its siloxane bond can form cross-linking system in fabric face hydrolysis, and organosilane monomer itself is also a kind of strong-hydrophobicity monomer, which not only improves the water-fast of fabric, resistance toheat, and also improve flexibility and the smoothness of fabric, reduce the frictional coefficient of fabric face, thus substantially increase the crock fastness especially fastness to wet rubbing of fabric, in addition, the quaternary ammonium salt cationic group in product structure of the present invention, it has stronger polarity, and can form insoluble dye salt with the anionic reactive of dyestuff and precipitate, the dyestuff on further fixed fabric, reaches the object of further fixation.Triple fixation makes fabric fastness better, has more the performances such as water-fastness, rub resistance.
The product utilizing the present invention to obtain is that one does not contain formaldehyde, the novel dyeing and printing auxiliary of green nontoxic, harmless, safe and reliable, free from environmental pollution.
Embodiment
Describe embodiments of the present invention in detail below with reference to specific embodiment, to the present invention, how utilisation technology means solve technical problem whereby, and the implementation procedure reaching technique effect can fully understand and implement according to this.
If do not specialize, the conventional means that the technique means adopted in embodiment is well known to those skilled in the art, the reagent adopted and product be also can business obtain.Source, the trade(brand)name of agents useful for same and be necessary to list its moiety person, all indicate when occurring first.
Embodiment one
A kind of cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent and preparation method thereof, comprises the following steps:
(1) in reactor, add 0.2 kilogram of disodium ethylene diamine tetraacetate and 2 kilograms of described deionized waters, open and stir, stir after dissolving completely, add again from two header tanks simultaneously, what drip in the first header tank be 350 kilogram-mass percentage concentrations is the dimethyl diallyl ammonium chloride of 60%, what drip in the second header tank is 89 kg ethylene base Trimethoxy silanes, mixing and stirring;
(2) with the speed of 50mL/min logical nitrogen 60min in reactor, and heat temperature raising is started;
(3) when temperature is raised to 60 DEG C, drip from the 3rd header tank, what drip in the 3rd header tank be 40 kilogram-mass percentage concentrations is the initiator solution of 2%, and it is formulated that this initiator solution adds 39.2 kilograms of deionized waters by 0.8 kilogram of described ammonium persulphate; Time for adding controls 1.0 hours (that is, controlling to drip speed makes it drip off at 1.0 hours), and dropping temperature controls at 65 DEG C;
(4) drip rear maintenance temperature and continue reaction 2.0 hours, then add deionized water again by product requirement and dilute, after stirring, obtain cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent.
Embodiment two
A kind of cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent and preparation method thereof, comprises the following steps:
(1) in reactor, add 0.4 kilogram of Sunmorl N 60S and 2 kilograms of deionized waters, open and stir, stir after dissolving completely, add again from two header tanks simultaneously, what add in the first header tank is 400 kilograms of dimethyl diallyl ammonium chlorides, what add in the second header tank is 59 kg ethylene ethyl triethoxy silicane alkane, mixing and stirring;
(2) with the speed of 80mL/min logical nitrogen 45min in reactor, and heat temperature raising is started;
(3) when temperature is raised to 65 DEG C, drip from the 3rd header tank, the 3rd header tank is 20 kilogram-mass percentage concentrations is the initiator solution of 3%, and it is formulated that this initiator solution adds 19.4 kilograms of deionized waters by 0.6 kilogram of ammonium persulphate.Time for adding controls 1.5 hours (that is, controlling to drip speed makes it drip off at 1.5 hours), and dropping temperature controls at 70 DEG C;
(4) drip rear maintenance temperature and continue reaction 2.5 hours, then add deionized water again by product requirement and dilute, after stirring, obtain cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent.
Embodiment three
A kind of cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent and preparation method thereof, comprises the following steps:
(1) in reactor, add 0.5 kilogram of tetrasodium ethylenediamine tetraacetate and 2 kilograms of deionized waters, open and stir, stir after dissolving completely, add again from two header tanks simultaneously, what add in the first header tank is 450 kilograms of dimethyl diallyl ammonium chlorides, what add in the second header tank is 29 kg ethylene base triacetoxysilanes, mixing and stirring;
(2) with the speed of 100mL/min logical nitrogen 40min in reactor, and heat temperature raising is started;
(3) when temperature is raised to 65 DEG C, drip from the 3rd header tank, 3rd header tank is 25 kilogram-mass percentage concentrations is the initiator solution of 2%, this initiator solution by 0.5 kilogram of described Potassium Persulphate and 24.5 kilograms of described deionized waters formulated, at 2.0 hours (namely time for adding controls, controlling to drip speed makes it drip off at 2.0 hours), dropping temperature controls at 70 DEG C;
(4) drip rear maintenance temperature and continue reaction 3.0 hours, then add deionized water again by product requirement and dilute, after stirring, obtain cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent.
Embodiment four
A kind of cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent and preparation method thereof, comprises the following steps:
(1) in reactor, add 0.6 kilogram of tripoly phosphate sodium STPP and 2 kilograms of deionized waters, open and stir, stir after dissolving completely, add again from two header tanks simultaneously, what add in the first header tank is 460 kilograms of dimethyl diallyl ammonium chlorides, what add in the second header tank is 21.6 kg ethylene base three ('beta '-methoxy oxyethyl group) silane, mixing and stirring;
(2) with the speed of 120mL/min logical nitrogen 30min in reactor, and heat temperature raising is started;
(3) when temperature is raised to 65 DEG C, drip from the 3rd header tank, what the 3rd header tank dripped is 36 kilogram-mass percentage concentrations is the initiator solution of 5%, this initiator solution is formulated by 0.9 kilogram of described ammonium persulphate, 0.9 kilogram of Sodium Persulfate and 34.2 kilograms of deionized waters, at 1.5 hours (namely time for adding controls, controlling to drip speed makes it drip off at 1.5 hours), dropping temperature controls at 70 DEG C;
(4) drip rear maintenance temperature and continue reaction 3.0 hours, then add deionized water again by product requirement and dilute, after stirring, obtain cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent.
Embodiment five
A kind of cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent and preparation method thereof, comprises the following steps:
(1) in reactor, add 0.8 kilogram of Trisodium Citrate and 2 kilograms of deionized waters, open and stir, stir after dissolving completely, add again from two header tanks simultaneously, what add in the first header tank is 470 kilograms of dimethyl diallyl ammonium chlorides, what add in the second header tank is 14.6 kilograms of methacryloxypropyl trimethoxy silane, mixing and stirring;
(2) with the speed of 160mL/min logical nitrogen 20min in reactor, and heat temperature raising is started;
(3) when temperature is raised to 70 DEG C, drip from the 3rd header tank, what drip in the 3rd header tank be 32.5 kilogram-mass percentage concentrations is the initiator solution of 8%, this initiator solution is formulated by 1.3 kilograms of ammonium persulphates, 1.3 kilograms of Potassium Persulphates and 29.9 kilograms of deionized waters, at 2.0 hours (namely time for adding controls, controlling to drip speed makes it drip off at 2.0 hours), dropping temperature controls at 75 DEG C;
(4) drip rear maintenance temperature and continue reaction 3.5 hours, then add deionized water again by product requirement and dilute, after stirring, obtain cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent.
Embodiment six
A kind of cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent and preparation method thereof, comprises the following steps:
(1) in reactor, add 0.9 kilogram of tetrasodium ethylenediamine tetraacetate and 2 kilograms of deionized waters, open and stir, stir after dissolving completely, add again from two header tanks simultaneously, what add in the first header tank is 480 kilograms of dimethyl diallyl ammonium chlorides, what add in the second header tank is 8.2 kilograms of t etram-ethyltetravinylcyclotetrasiloxane, mixing and stirring;
(2) with the speed of 200mL/min logical nitrogen 10min in reactor, and heat temperature raising is started;
(3) when temperature is raised to 75 DEG C, drip from the 3rd header tank, what drip in the 3rd header tank be 58 kilogram-mass percentage concentrations is the initiator solution of 5%, this initiator solution is formulated by the described deionized water of 1.45 kilograms of Sodium Persulfates, 1.45 kilograms of Potassium Persulphates and 55.1 kilograms, at 1.5 hours (namely time for adding controls, controlling to drip speed makes it drip off at 1.5 hours), dropping temperature controls at 80 DEG C;
(4) drip rear maintenance temperature and continue reaction 4.0 hours, then add deionized water again by product requirement and dilute, after stirring, obtain cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent.
Cotton fabric after the bright red 4BS dyeing of the cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent process that above-described embodiment 1 ~ 6 is prepared, adopt padding process, technical process is:
DYED FABRICS → pad laking agent working fluid (pick-up 85%) → oven dry (130 DEG C, 3min).
Elevator working solution concentration is 15g/L, pH is 6 ~ 7.Salient features (dyefastness) after Cotton Fabric is shown in Table 1.
the main performance index of table 1 cotton fabric after above-described embodiment 1 ~ 6 fixation treatment
Remarks:
1. crock fastness testing method presses GB/T3920-2008 " textile color stability test colour fastness to rubbing " method mensuration;
2. soaping fastness testing method presses GB/T3921-2008 " textile color stability test colour fastness to washing " method mensuration;
3. color fixing agent Y is commercially available.
The cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent adopting method of the present invention to prepare has higher positive charge density, ionic linkage can be combined into the negative charge of cellulose fiber peacekeeping dyestuff, the siloxane structure simultaneously introduced, its siloxane bond can form cross-linking system in fabric face hydrolysis, and organosilane monomer itself is also a kind of strong-hydrophobicity monomer, which not only improves the water-fast of fabric, resistance toheat, and also improve flexibility and the smoothness of fabric, reduce the frictional coefficient of fabric face, thus substantially increase the crock fastness especially fastness to wet rubbing of fabric, in addition, the quaternary ammonium salt cationic group in product structure of the present invention, it has stronger polarity, and can form insoluble dye salt with the anionic reactive of dyestuff and precipitate, the dyestuff on further fixed fabric, reaches the object of further fixation.Triple fixation makes fabric fastness better, has more the performances such as water-fastness, rub resistance.
The product utilizing the present invention to obtain is that one does not contain formaldehyde, the novel dyeing and printing auxiliary of green nontoxic, harmless, safe and reliable, free from environmental pollution.
Claims (5)
1. a preparation method for cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent, is characterized in that, comprise the steps:
(1) by percentage to the quality, first sequestrant and the deionized water of 0.02 ~ 0.2 weight part is added in a kettle., be mixed with the chelating agent solution that mass percent concentration is 5% ~ 35%, stir after dissolving completely, add the dimethyl diallyl ammonium chloride of 35 ~ 49 weight parts and the organosilane monomer of 0.5 ~ 12 weight part again, mixing and stirring obtains mixing solutions; Described organosilane monomer is vinyltrimethoxy silane, vinyltriethoxysilane, vinyltriacetoxy silane, vinyl three ('beta '-methoxy oxyethyl group) silane, methacryloxypropyl trimethoxy silane, tetramethyl divinyl disiloxane, t etram-ethyltetravinylcyclotetrasiloxane or vinyl tributyl ketoximyl silane;
(2) secondly, in reactor, lead to nitrogen 10 ~ 60 minutes with the speed of 50mL/min ~ 200mL/min, and start heat temperature raising;
(3) when temperature rises to 60 ~ 80 DEG C, then drip the initiator solution that mass percent concentration is 0.05 ~ 0.2 weight part of 1 ~ 10%, time for adding controls at 0.5 ~ 2 hour;
(4) polyreaction is carried out after dropwising, controlling the reaction times is 2 ~ 5 hours, finally add deionized water according to product requirement to carry out being diluted to setting concentration, after stirring, namely obtain cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent.
2. the preparation method of a kind of cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent according to claim 1, is characterized in that: in described step (1) sequestrant be in tripoly phosphate sodium STPP, Sodium hexametaphosphate 99, Trisodium Citrate, sodium tartrate, Sunmorl N 60S, disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate, nitrilotriacetic acid sodium, cyclohexanediaminetetraacetic acid sodium, diethylene triamine pentacetic acid (DTPA) sodium any one or two or more with arbitrarily than the mixture of mixing.
3. the preparation method of a kind of cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent according to claim 1 and 2, is characterized in that: the aqueous solution of dimethyl diallyl ammonium chloride to be mass percent concentration be 60 ± 0.5% or 65 ± 0.5% in described step (1).
4. the preparation method of a kind of cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent according to claim 1, is characterized in that: the nitrogen in described step (2) is liquid nitrogen or the nitrogen of gaseous state.
5. the preparation method of a kind of cation type organic silicon modified Poly Dimethyl Diallyl Ammonium Chloride laking agent according to claim 1, is characterized in that: in described step (3) initiator be in ammonium persulphate, Sodium Persulfate, Potassium Persulphate any one or two or more with arbitrarily than the mixture of mixing.
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| CN104744641B (en) * | 2015-03-09 | 2018-04-17 | 浙江工业职业技术学院 | A kind of cation formaldehyde-free color fixing agent lotion |
| CN105727903B (en) * | 2016-02-17 | 2018-01-30 | 济南大学 | A kind of modified porous diatomaceous preparation method of dimethyl diallyl ammonium chloride |
| CN105755870A (en) * | 2016-02-26 | 2016-07-13 | 苏州三和开泰花线织造有限公司 | Alkali-resistant chlorine-resistant type aldehyde-free active dye color fixing agent and preparation method thereof |
| CN105862476B (en) * | 2016-05-20 | 2017-12-22 | 刘剑锋 | A kind of formaldehyde-free active dye fixing agent and preparation method thereof |
| CN108660813A (en) * | 2018-07-07 | 2018-10-16 | 曾文华 | A kind of formaldehyde-free color fixing agent and preparation method thereof |
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| CN110092870B (en) * | 2019-04-08 | 2021-03-16 | 佛山市晟世纺织科技有限公司 | Dye binder composition |
| CN112813710B (en) * | 2020-12-31 | 2021-12-14 | 珠海华大浩宏新材料有限公司 | Energy-saving and water-saving dyeing post-treatment auxiliary agent and preparation method thereof |
| CN113605082A (en) * | 2021-07-30 | 2021-11-05 | 奥仕集团有限公司 | Method for preventing dye from fading by using fluorescent whitening slurry |
| CN113637127A (en) * | 2021-08-16 | 2021-11-12 | 广东传化富联精细化工有限公司 | Color fixing agent for cotton for after-finishing and preparation method thereof |
| CN115852719B (en) * | 2022-09-30 | 2024-03-26 | 浙江越新印染有限公司 | Silicon-containing color fixing auxiliary agent and application thereof in cotton printing and dyeing |
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