A kind of formaldehyde-free active dye fixing agent and preparation method thereof
Technical field
The invention belongs to field of fine chemical, particularly to a kind of formaldehyde-free active dye fixing agent and preparation method thereof.
Background technology
Reactive dye are cheap, chromatogram is complete, bright in colour, be widely used in cotton fabric dyeing process.Although reactive dye
Reactive group in molecule is easily combined with covalent bond with fiber, but color fastness is unsatisfactory.It is in dyeing course, particularly
When dye is dark, often there are the reactive dye making to there is a large amount of non-set on dyed fabric because dye strength is too high, these
The dyestuff of non-set is difficult to eccysis from dyed fabric, and this some dyes will fade in washing process;Meanwhile, some activity
The chemical bond facile hydrolysis formed between base and fiber, causes wet colour fastness relatively low.And color fixing agent such as color fixing agent Y in early days is first
The product of the reaction such as aldehyde, dicyandiamide and ammonium chloride, although every fastness of product dyed thereby can be improved, but there is content of formaldehyde relatively
Height, the problem such as be detrimental to health, and has not met International Textile requirement.Along with constantly expanding and people of World Textile trade
People's living standard, the improving constantly of environmental consciousness, propose higher requirement to indexs such as comfortable, cleaning, the safety of textile.
Since entering 21 century, World Textile Market fastness every to product dyed thereby is had higher requirement, through fixation
Agent process after product dyed thereby, not only to have the soaping of certain grade, wash, rub resistance, perspiration resistance, the jail such as sun-resistant, chlorine-resistant drift
Degree, but also require without formaldehyde, nontoxic, do not affect fabric feeling and discoloration etc..Therefore, research meets ecological, environmental protective, Wu Jia
The new reactive dyes color fixing agent of aldehyde is a significant job.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of formaldehyde-free active dye fixing agent and system thereof
Preparation Method, this color fixing agent can more preferably improve fabric fastness to wet rubbing and color fastness to washing and without formaldehyde.
To achieve these goals, the present invention is by the following technical solutions:
A kind of preparation method of formaldehyde-free active dye fixing agent, including the raw material components of following portions by weight proportioning:
Described silicon-containing monomer is vinyl three (2-methoxy ethoxy) silane, 3-(methacryloxypropyl) propyl group trimethoxy
In base silane, 3-(methacryloxypropyl) hydroxypropyl methyl dimethoxysilane any one or two or more with any than mixing
Mixture.
Described chelating agent be poly-epoxy succinic acid or poly-aspartate or both with any than mixing mixture.
Described initiator be in ammonium persulfate, sodium peroxydisulfate and potassium peroxydisulfate any one or two or more with arbitrarily than
The mixture of mixing.
The preparation method of a kind of formaldehyde-free active dye fixing agent, is achieved by the steps of:
(1) equipped with thermometer, agitator, reflux condenser reactor in be sequentially added into described oleic imidazolinone quaternary ammonium
Returned cold is opened after salt, trimethyolol propane monoallyl ether, 1,3-diallyl urea, silicon-containing monomer, chelating agent, deionized water
Solidifying, stirring, and begin to warm up intensification;
(2) when temperature rises to 85~100 DEG C, then start to drip mass percent concentration be 1~10% initiator molten
Liquid, this initiator solution is formulated by the described deionized water of described initiator and part;Time for adding controls in 0.5~4 little
Time, during dropping, temperature controls at 85~100 DEG C;
(3) insulation reaction 1~5 hours again after adding, be subsequently added into the water of surplus, and discharging after stirring 0.5 hour obtains institute
State color fixing agent.
Compared with prior art, the present invention has a following remarkable result:
1, by introduce amino, ether, containing silicon structure isoreactivity group, make color fixing agent in use, can be with dye
Material, the active group (such as hydroxyl, amino etc.) of fiber molecule crosslink combination, thus reduce the dyestuff compatibility to water, carry
The wet colour fastnesses such as the soaping of high dyed fabric, staining.Additionally, molecule has quaternary ammonium salt cationic group, pass through cation
, there is Coulomb attraction effect, neutralize its electric charge in the anion such as the sulfonic group of base and reactive dye (including its hydrolised dye), reduces
The water solubility of dyestuff, and be combined with dye anion, increase the active force between dye molecule and fiber molecule, to improve wet jail
Degree.
2, the formaldehydeless pollution of prepared color fixing agent, effectively reduces fabric formaldehyde content, promotes the quality of fabric, meets
Environmental requirement and the health demand of the people, have wide market prospects.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further elaborated on.
A kind of formaldehyde-free active dye fixing agent of the present invention, is made up of the raw material components of following portions by weight proportioning:
Described silicon-containing monomer is vinyl three (2-methoxy ethoxy) silane, 3-(methacryloxypropyl) propyl group trimethoxy
Any one or two kinds in base silane, 3-(methacryloxypropyl) hydroxypropyl methyl dimethoxysilane are with any mixed than mixing
Compound.
Described chelating agent is in poly-epoxy succinic acid or poly-aspartate or both are with any mixture than mixing.
Described initiator be in ammonium persulfate, sodium peroxydisulfate or potassium peroxydisulfate any one or two or more with arbitrarily than
The mixture of mixing.
The preparation method of a kind of formaldehyde-free color fixing agent for reactive dyes of the present invention, is achieved by the steps of:
(1) equipped with thermometer, agitator, reflux condenser reactor in be sequentially added into described oleic imidazolinone quaternary ammonium
Returned cold is opened after salt, trimethyolol propane monoallyl ether, 1,3-diallyl urea, silicon-containing monomer, chelating agent, deionized water
Solidifying, stirring, and begin to warm up intensification;
(2) when temperature rises to 85~100 DEG C, then start to drip mass percent concentration be 1~10% initiator molten
Liquid, this initiator solution is formulated by the described deionized water of described initiator and part;Time for adding controls in 0.5~4 little
Time, during dropping, temperature controls at 85~100 DEG C;
(3) insulation reaction 1~5 hours again after adding, be subsequently added into the water of surplus, and discharging after stirring 0.5 hour obtains institute
State color fixing agent.
With specific embodiment, the present invention is described in detail below, but the present invention is not limited only to this.
Embodiment one
A kind of formaldehyde-free active dye fixing agent of the present invention, is made up of the raw material components of following portions by weight proportioning:
Its preparation method, is achieved by the steps of:
(1) equipped with thermometer, agitator, reflux condenser reactor in be sequentially added into 22 parts of oleic imidazolinone quaternary ammoniums
Salt, 2 parts of trimethyolol propane monoallyl ether, 18 parts of 1,3-diallyl ureas, 4 parts of vinyl three (2-methoxy ethoxy) silicon
Open reflux condensation mode, stirring after alkane, 1 part of poly-aspartate, 20 parts of deionized waters, and begin to warm up intensification;
(2), when temperature rises to 98 DEG C, then start to drip the ammonium persulfate solution that mass percent concentration is 5%, this mistake
Ammonium sulfate is formulated by 1 part of ammonium persulfate and 19 parts of deionized waters;Time for adding controls at 2 hours, temperature during dropping
Control at 98 DEG C;
(3) insulation reaction 4 hours again after adding, are subsequently added into the water of surplus, discharging after stirring 0.5 hour, obtain described
Color fixing agent.
Embodiment two
A kind of formaldehyde-free active dye fixing agent of the present invention, is made up of the raw material components of following portions by weight proportioning:
Its preparation method, is achieved by the steps of:
(1) equipped with thermometer, agitator, reflux condenser reactor in be sequentially added into 25 parts of oleic imidazolinone quaternary ammoniums
Salt, 4 parts of trimethyolol propane monoallyl ether, 16 parts of 1,3-diallyl ureas, 8 parts of 3-(methacryloxypropyl) propyl group trimethoxies
Open reflux condensation mode, stirring after base silane, 1 part of poly-aspartate, 10 parts of deionized waters, and begin to warm up intensification;
(2), when temperature rises to 95 DEG C, then start to drip the sodium peroxydisulfate solution that mass percent concentration is 2%, this mistake
Metabisulfite solution is formulated by 0.5 part of sodium peroxydisulfate and 24.5 parts of deionized waters;Time for adding controls at 3 hours, during dropping
Temperature controls at 97 DEG C;
(3) insulation reaction 4 hours again after adding, are subsequently added into the water of surplus, discharging after stirring 0.5 hour, obtain described
Color fixing agent.
Embodiment three
A kind of formaldehyde-free active dye fixing agent of the present invention, is made up of the raw material components of following portions by weight proportioning:
Its preparation method, is achieved by the steps of:
(1) equipped with thermometer, agitator, reflux condenser reactor in be sequentially added into 25 parts of oleic imidazolinone quaternary ammoniums
Salt, 6 parts of trimethyolol propane monoallyl ether, 14 parts of 1,3-diallyl ureas, 6 parts of 3-(methacryloxypropyl) hydroxypropyl methyl two
Open reflux condensation mode, stirring after methoxy silane, 2 parts of poly-epoxy succinic acids, 12 parts of deionized waters, and begin to warm up intensification;
(2), when temperature rises to 90 DEG C, then start to drip the sodium peroxydisulfate solution that mass percent concentration is 4%, this mistake
Metabisulfite solution is formulated by 1 part of sodium peroxydisulfate and 24 parts of deionized waters;Time for adding controls at 3.5 hours, temperature during dropping
Degree controls at 93 DEG C;
(3) insulation reaction 4.5 hours again after adding, are subsequently added into the water of surplus, and discharging after stirring 0.5 hour obtains institute
State color fixing agent.
Embodiment four
A kind of formaldehyde-free active dye fixing agent of the present invention, is made up of the raw material components of following portions by weight proportioning:
Its preparation method, is achieved by the steps of:
(1) equipped with thermometer, agitator, reflux condenser reactor in be sequentially added into 30 parts of oleic imidazolinone quaternary ammoniums
Salt, 8 parts of trimethyolol propane monoallyl ether, 12 parts of 1,3-diallyl ureas, 7 parts of 3-(methacryloxypropyl) hydroxypropyl methyl two
Open reflux condensation mode, stirring after methoxy silane, 2.5 parts of poly-epoxy succinic acids, 10 parts of deionized waters, and begin to warm up intensification;
(2), when temperature rises to 97 DEG C, then start to drip the potassium persulfate solution that mass percent concentration is 5%, this mistake
Potassium sulfate solution is formulated by 1 part of potassium peroxydisulfate and 19 parts of deionized waters;Time for adding controls at 2.5 hours, temperature during dropping
Degree controls at 98 DEG C;
(3) insulation reaction 2.5 hours again after adding, are subsequently added into the water of surplus, and discharging after stirring 0.5 hour obtains institute
State color fixing agent.
Embodiment five
A kind of formaldehyde-free active dye fixing agent of the present invention, is made up of the raw material components of following portions by weight proportioning:
Wherein:
Silicon-containing monomer uses vinyl three (2-methoxy ethoxy) silane and 3-(methacryloxypropyl) propyl group trimethoxy
The mixture of base silane, and vinyl three (2-methoxy ethoxy) silane and 3-(methacryloxypropyl) propyl trimethoxy silicon
The amount ratio of alkane is 1:1, i.e. vinyl three (2-methoxy ethoxy) silane and 3-(methacryloxypropyl) propyl trimethoxy
The consumption of silane is respectively 4 parts and 4 parts.
Its preparation method, is achieved by the steps of:
(1) equipped with thermometer, agitator, reflux condenser reactor in be sequentially added into 35 parts of oleic imidazolinone quaternary ammoniums
Salt, 10 parts of trimethyolol propane monoallyl ether, 10 parts of 1,3-diallyl ureas, 4 parts of vinyl three (2-methoxy ethoxy)
Open back after silane, 4 parts of 3-(methacryloxypropyl) propyl trimethoxy silicanes, 1.5 parts of poly-aspartates, 8 parts of deionized waters
Stream condensation, stirring, and begin to warm up intensification;
(2), when temperature rises to 92 DEG C, then start to drip the ammonium persulfate solution that mass percent concentration is 5%, this mistake
Ammonium sulfate is formulated by 1 part of ammonium persulfate and 19 parts of deionized waters;Time for adding controls at 3 hours, temperature during dropping
Control at 99 DEG C;
(3) insulation reaction 4 hours again after adding, are subsequently added into the water of surplus, discharging after stirring 0.5 hour, obtain described
Color fixing agent.
Embodiment six
A kind of formaldehyde-free active dye fixing agent of the present invention, is made up of the raw material components of following portions by weight proportioning:
Wherein:
Silicon-containing monomer uses vinyl three (2-methoxy ethoxy) silane and 3-(methacryloxypropyl) hydroxypropyl methyl two
The mixture of methoxy silane, and vinyl three (2-methoxy ethoxy) silane and 3-(methacryloxypropyl) hydroxypropyl methyl two
The amount ratio of methoxy silane is 1:2, i.e. vinyl three (2-methoxy ethoxy) silane and 3-(methacryloxypropyl) propyl group
The consumption of methyl dimethoxysilane is respectively 3 parts and 6 parts.
Initiator uses sodium peroxydisulfate and the mixture of potassium peroxydisulfate, and the amount ratio of sodium peroxydisulfate and potassium peroxydisulfate is 1:
2, i.e. the consumption of sodium peroxydisulfate and potassium peroxydisulfate is 0.5 part and 1 part.
Its preparation method, is achieved by the steps of:
(1) equipped with thermometer, agitator, reflux condenser reactor in be sequentially added into 38 parts of oleic imidazolinone quaternary ammoniums
Salt, 12 parts of trimethyolol propane monoallyl ether, 8 parts of 1,3-diallyl ureas, 3 parts of vinyl three (2-methoxy ethoxy) silicon
Open after alkane, 6 parts of 3-(methacryloxypropyl) hydroxypropyl methyl dimethoxysilane, 2 parts of poly-epoxy succinic acids, 3 parts of deionized waters
Reflux condensation mode, stirring, and begin to warm up intensification;
(2) when temperature rises to 95 DEG C, then starting to drip the initiator solution that mass percent concentration is 6%, this causes
Agent solution is formulated by 0.5 part of sodium peroxydisulfate and 1 part of potassium peroxydisulfate and 23.5 parts of deionized waters;Time for adding controls 3 little
Time, during dropping, temperature controls at 97 DEG C;
(3) insulation reaction 3 hours again after adding, are subsequently added into the water of surplus, discharging after stirring 0.5 hour, obtain described
Color fixing agent.
The color fixing agent that above-described embodiment one to six directions becomes is processed respectively the bafta after reactive scarlet 3 grams dyeing, uses
The solid technique of leaching, color fixing agent consumption is 2% (o.w.f), and pH is 6~7, and temperature is 60 DEG C, and the time is 30min, bath raio 1:12.Cotton is knitted
Main performance index after thing fixation is as shown in table 1.
Table 1 bafta main performance index after above-described embodiment one to six fixation treatment
Remarks:
1. crock fastness method of testing presses GB/T3920-2008 " textile color stability test colour fastness to rubbing " method
Measure;
2. soaping fastness method of testing presses the survey of GB/T3921-2008 " textile color stability test color fastness to washing " method
Fixed;
3. sweat leaching fastness method of testing presses the survey of GB/T5713-2013 " textile color stability test color fastness to water " method
Fixed.
4. control sample is the aldehyde-free colour stabilizer that Guangzhou Zhuan Jie Chemical Co., Ltd. produces, and concentration is 30%.
Described above, only utilize the embodiment of this origination techniques content, any those skilled in the art to use this wound
Make modification, the change done, all belong to the scope of the claims that this creation is advocated, and be not limited to those disclosed embodiments.