CN105175631B - A kind of preparation method of reactive dye cationic formaldehyde-free fixing agent - Google Patents
A kind of preparation method of reactive dye cationic formaldehyde-free fixing agent Download PDFInfo
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Abstract
The reactive dye cationic formaldehyde-free fixing agent of fabric fastness to wet rubbing and color fastness to washing can be more preferably improved there is provided a kind of the present invention relates to color fixing agent technical field, the raw material components matched by following mass fractions are made：50~60 parts of dimethyl diallyl ammonium chloride；0.2~10 part of tertiary-amino-containing monomer；0.1~5 part of crosslinking agent；0.01~0.3 part of initiator；30~48 parts of deionized water；Wherein, the dimethyl diallyl ammonium chloride is the aqueous solution that mass percent concentration is 60 ± 0.5% or 65 ± 0.5%；There is provided a kind of preparation method of the reactive dye cationic formaldehyde-free fixing agent simultaneously.
Description
Technical field
The present invention relates to color fixing agent technical field, more particularly to a kind of system of reactive dye cationic formaldehyde-free fixing agent
Preparation Method.
Background technology
At present, textile dyeing is mainly based on reactive dyeing, but during dyeing and printing process, reactive dye and fiber
The bonding reaction and hydrolysis of cellulose fiber are simultaneous, and the presence of hydrolysis causes reactive dye color fixing rate relatively
It is low；Moreover, often occurring because dense during dyeing containing hydrophilic radicals such as sulfonic group, carboxylic acid groups in reactive dyestuff molecule structure
Spend high and the amount of dye of its set is limited, cause dyeing unqualified, dyed fabric fastness to wet rubbing especially in, deep-colour fabric
Fastness to wet rubbing it is relatively low, therefore fabric also carries out fixation treatment after dyeing process with color fixing agent.
In addition, with the continuous enhancing of environmental consciousness, dyeing assistant is constantly to environmental protection, energy-efficient direction hair
The color fixing agent of exhibition, no aldehyde or low aldehyde turns into the Main way of development and application.PDDA color fixing agent conduct
The ideal quaternary ammonium salt Polycationic aldehyde-free colour stabilizer of one class, meets new environmental requirement and constantly attracts attention.But because
The ionic bond effect of itself and dyestuff and the van der Waals interaction between cotton-textile fibres in the presence of the external force such as friction easily by
To destruction, and make it that fastness to wet rubbing is undesirable.For this case, the structure to PDDA is carried out
It is modified, new active group is introduced, then can effectively improve its color fixation fastness.
The content of the invention
Therefore, for above content, the present invention, which provides one kind, can more preferably improve fabric fastness to wet rubbing and color fastness to washing
Reactive dye cationic formaldehyde-free fixing agent, while providing a kind of reactive dye cationic formaldehyde-free fixing agent
Preparation method.
To reach above-mentioned purpose, the present invention is achieved by the following technical solutions：A kind of reactive dye cationic
Aldehyde-free colour stabilizer, the raw material components matched by following mass fractions are made：
Wherein, the dimethyl diallyl ammonium chloride is that mass percent concentration is 60 ± 0.5% or 65 ± 0.5%
The aqueous solution.
Further improving is：Each raw material and its content are：
Further improving is：The tertiary-amino-containing monomer is dimethylaminoethyl acrylate, acrylate third
Ester, dimethylaminoethyl acrylate, dimethylaminoethyl methacrylate, dimethylaminoethyl propyl ester and metering system
Any one in sour lignocaine propyl ester or or the two or more mixtures with any ratio mixing.
Further improving is：The crosslinking agent is in diallylamine, triallylamine, N- amide
Any one is two or more with any mixture than mixing.
Further improving is：The initiator be ammonium persulfate, sodium peroxydisulfate or potassium peroxydisulfate in any one or
The two or more mixtures with any ratio mixing.
A kind of preparation method of reactive dye cationic formaldehyde-free fixing agent, comprises the following steps：
(1) toward 50~60 parts by weight dimethyl diallyl ammonium chlorides of addition in reactor, stirring is opened, and begin to warm up
Heating；
(2) when temperature rises to 60~90 DEG C, it is added dropwise simultaneously from two head tanks, 0.2~10 is added dropwise in the first head tank
Parts by weight tertiary-amino-containing monomer, it is 1~10% that the mass percent concentration of 0.01~0.3 parts by weight, which is added dropwise, in the second head tank
Initiator solution, time for adding control was at 0.5~3 hour, and dropping temperature is controlled at 65~95 DEG C；
(3) drip rear keeping temperature to continue to react 1~3 hour, then add 0.1~5 parts by weight of crosslinking agent, keep temperature
Degree continues to react 0.5~3 hour, adds deionized water and is diluted, after stirring, produces reactive dye cationic
Aldehyde-free colour stabilizer.
By using preceding solution, the beneficial effects of the invention are as follows：
1st, can be with dye by introducing tertiary amino, ester group isoreactivity group in color fixing agent structure, and with cationic properties
Expect the reactive group of molecule, the hydroxyl crosslinking on cellulosic molecule, form height diversification interconnected system, make dyestuff and fiber
With reference to more firmly, so as to significantly improve the dry fastness, fastness to wet rubbing and color fastness to washing of reactive dye, and
The coloured light and feel of product are not influenceed.
2nd, make prepared fixation agent molecule that network structure is presented by crosslinking, film forming is strong.After drying processing, knitting
Thing surface forms soft, tough and tensile film.
3rd, prepared color fixing agent has dyefastness high, can improve dry and wet fastness, Washing, formaldehydeless pollution,
Fabric formaldehyde content is effectively reduced, the quality of fabric is lifted, environmental protection, pollution are small, with wide market prospects.
Embodiment
Describe embodiments of the present invention in detail below with reference to specific embodiment, how skill is applied to the present invention whereby
Art means solve technical problem, and reach the implementation process of technique effect and can fully understand and implement according to this.
Unless otherwise specified, the conventional hand that the technological means employed in embodiment is well known to those skilled in the art
Section, the reagent and product used is also available commercial.The source of agents useful for same, trade name and it is necessary to list it
Constituent person, indicates on the first appearance.
Embodiment one
A kind of reactive dye cationic formaldehyde-free fixing agent, is made up of the raw material components of following mass parts：
Dimethyl diallyl ammonium chloride：508 kilograms
Dimethylaminoethyl acrylate：13 kilograms
Diallylamine：8kg
Ammonium persulfate：0.2 kilogram
Deionized water：470.8 kilogram；
Wherein, dimethyl diallyl ammonium chloride is the aqueous solution that mass percent concentration is 60%.
Its preparation method, comprises the following steps：
(1) toward the dimethyl diallyl ammonium chloride of 508 kilograms of addition in reactor, stirring is opened, and begin to warm up liter
Temperature；
(2) when temperature rises to 68 DEG C, it is added dropwise simultaneously from two head tanks, the first head tank is 13 kilograms of acrylic acid two
The ammonium persulfate solution that 4 kilogram-mass percent concentrations are 5% is added dropwise in methylamino ethyl ester, the second head tank, and this ammonium persulfate is molten
Liquid adds 3.8 kilograms of deionized waters by 0.2 kilogram of ammonium persulfate and is formulated.Time for adding control (that is, was controlled at 2 hours
System drop speed makes it be dripped off at 2 hours), dropping temperature is controlled at 70 DEG C；
(3) drip rear keeping temperature to continue to react 2 hours, then add 8 kilograms of diallylamine, keeping temperature after
Continuous reaction 1.5 hours, adds the remaining deionized water and is diluted, after stirring, produce reactive dye it is positive from
Subtype aldehyde-free colour stabilizer.
Embodiment two
A kind of reactive dye cationic formaldehyde-free fixing agent, is made up of the raw material components of following mass parts：
Dimethyl diallyl ammonium chloride：512 kilograms
Dimethylaminoethyl methacrylate：20 kilograms
Triallylamine：6 kilograms
Sodium peroxydisulfate：1.5 kilogram
Deionized water：460.5 kilogram；
Wherein, dimethyl diallyl ammonium chloride is the aqueous solution that mass percent concentration is 65%.
Its preparation method, comprises the following steps：
(1) toward the dimethyl diallyl ammonium chloride of 512 kilograms of addition in reactor, stirring is opened, and begin to warm up liter
Temperature；
(2) when temperature rises to 75 DEG C, it is added dropwise simultaneously from two head tanks, the first head tank is 20 kilograms of acrylic acid two
The sodium peroxydisulfate solution that 20 kilogram-mass percent concentrations are 7.5%, this sodium peroxydisulfate is added dropwise in methylamino propyl ester, the second head tank
Solution adds 18.5 kilograms of deionized waters by 1.5 kilograms of sodium peroxydisulfates and is formulated, and time for adding was controlled at 2.5 hours
(that is, control drop speed makes it be dripped off at 2.5 hours), dropping temperature is controlled at 78 DEG C；
(3) drip rear keeping temperature to continue to react 2 hours, then add 6 kilograms of triallylamine, keeping temperature after
Continuous reaction 2 hours, adds the remaining deionized water and is diluted, after stirring, produce reactive dye cation
Type aldehyde-free colour stabilizer.
Embodiment three
A kind of reactive dye cationic formaldehyde-free fixing agent, is made up of the raw material components of following mass parts：
Dimethyl diallyl ammonium chloride：525 kilograms
Dimethylaminoethyl acrylate：25 kilograms
N- amides：25 kilograms
Potassium peroxydisulfate：1.8 kilogram
Deionized water：423.2 kilogram；
Wherein, dimethyl diallyl ammonium chloride is the aqueous solution that mass percent concentration is 60%.
Its preparation method, comprises the following steps：
(1) toward the dimethyl diallyl ammonium chloride of 525 kilograms of addition in reactor, stirring is opened, and begin to warm up liter
Temperature；
(2) when temperature rises to 80 DEG C, it is added dropwise simultaneously from two head tanks, the first head tank is 25 kilograms of acrylic acid two
The potassium persulfate solution that 25 kilogram-mass percent concentrations are 7.2%, this potassium peroxydisulfate is added dropwise in ethylamino propyl ester, the second head tank
Solution adds 23.2 kilograms of deionized waters by 1.8 kilograms of potassium peroxydisulfates and is formulated, and time for adding is controlled at 2 hours (i.e.,
Control drop speed makes it be dripped off at 2 hours), dropping temperature is controlled at 82 DEG C；
(3) drip rear keeping temperature to continue to react 1.5 hours, then add 25 kilograms of N- methyl diallyls, protect
Hold temperature to continue to react 2 hours, add the remaining deionized water and be diluted, after stirring, produce reactive dye
Use cationic formaldehyde-free fixing agent.
Example IV
A kind of reactive dye cationic formaldehyde-free fixing agent, is made up of the raw material components of following mass parts：
Dimethyl diallyl ammonium chloride：530 kilograms
Dimethylaminoethyl methacrylate：50 kilograms
N- amides：30 kilograms
Potassium peroxydisulfate：1 kilogram
Deionized water：389 kilograms；
Wherein, dimethyl diallyl ammonium chloride is the aqueous solution that mass percent concentration is about 65%.
Its preparation method, comprises the following steps：
(1) toward the dimethyl diallyl ammonium chloride of 530 kilograms of addition in reactor, stirring is opened, and begin to warm up liter
Temperature；
(2) when temperature rises to 85 DEG C, it is added dropwise simultaneously from two head tanks, 50 kilograms of methyl-prop is added dropwise in the first head tank
The potassium persulfate solution that 20 kilogram-mass percent concentrations are 5%, this over cure is added dropwise in olefin(e) acid dimethylaminoethyl, the second head tank
Sour potassium solution adds 19 kilograms of deionized waters by 1 kilogram of potassium peroxydisulfate and is formulated, and time for adding is controlled at 2 hours (i.e.,
Control drop speed makes it be dripped off at 2 hours), dropping temperature is controlled at 88 DEG C；
(3) drip rear keeping temperature to continue to react 1.5 hours, then add 30 kilograms of N- methyl diallyls, protect
Hold temperature to continue to react 2 hours, add the remaining deionized water and be diluted, after stirring, produce reactive dye
Use cationic formaldehyde-free fixing agent.
Embodiment five
A kind of reactive dye cationic formaldehyde-free fixing agent, the raw material components matched by following mass fractions are made：
Dimethyl diallyl ammonium chloride：550 kilograms
Dimethylaminoethyl propyl ester：70 kilograms
Diallylamine：30 kilograms
Potassium peroxydisulfate：1.6 kilogram
Deionized water：348.4 kilogram；
Wherein, dimethyl diallyl ammonium chloride is the aqueous solution that mass percent concentration is about 60%.
Its preparation method, comprises the following steps：
(1) toward the dimethyl diallyl ammonium chloride of 550 kilograms of addition in reactor, stirring is opened, and begin to warm up liter
Temperature；
(2) when temperature rises to 82 DEG C, it is added dropwise simultaneously from two head tanks, the first head tank is 70 kilograms of metering system
Sour dimethylamino propyl ester, the second head tank is the potassium persulfate solution that 32 kilogram-mass percent concentrations are 5%, this potassium peroxydisulfate
Solution adds 30.4 kilograms of deionized waters by 1.6 kilograms of potassium peroxydisulfates and is formulated, and time for adding is controlled at 2 hours (i.e.,
Control drop speed makes it be dripped off at 2 hours), dropping temperature is controlled at 85 DEG C；
(3) drip rear keeping temperature to continue to react 2 hours, then add 30 kilograms of diallylamine, keeping temperature
Continue to react 2 hours, add the remaining deionized water and be diluted, after stirring, produce reactive dye it is positive from
Subtype aldehyde-free colour stabilizer.
Embodiment six
A kind of reactive dye cationic formaldehyde-free fixing agent, is made up of the raw material components of following mass parts：
Dimethyl diallyl ammonium chloride：580 kilograms
Tertiary-amino-containing monomer：80 kilograms
Diallylamine：30 kilograms
Initiator：1 kilogram
Deionized water：309 kilograms；
Wherein：Dimethyl diallyl ammonium chloride is the aqueous solution that mass percent concentration is about 60%；
Tertiary-amino-containing monomer uses the mixing of dimethylaminoethyl propyl ester and methacrylic acid lignocaine propyl ester
Thing, and the mass ratio of dimethylaminoethyl propyl ester and methacrylic acid lignocaine propyl ester is 1:1, i.e. metering system
The consumption of sour dimethylamino propyl ester and methacrylic acid lignocaine propyl ester is 40 kilograms；
Initiator is using sodium peroxydisulfate and the mixture of potassium peroxydisulfate, and the mass ratio of sodium peroxydisulfate and potassium peroxydisulfate is 1:
1, i.e. the consumption of sodium peroxydisulfate and potassium peroxydisulfate is 0.5 kilogram.
Its preparation method, comprises the following steps：
(1) toward the dimethyl diallyl ammonium chloride of 580 kilograms of addition in reactor, stirring is opened, and begin to warm up liter
Temperature；
(2) when temperature rises to 77 DEG C, it is added dropwise simultaneously from two head tanks, the first head tank is 40 kilograms of metering system
The mixture of sour dimethylamino propyl ester and 40 kilograms of methacrylic acid lignocaine propyl ester, the second head tank is 20 kilogram-masses
Percent concentration is 5% sodium peroxydisulfate and potassium peroxydisulfate mixed solution, and this sodium peroxydisulfate solution is by 0.5 kilogram of persulfuric acid
Potassium and 0.5 kilogram of sodium peroxydisulfate add 19 kilograms of deionized waters and are formulated, and time for adding control (that is, was controlled at 1.5 hours
System drop speed makes it be dripped off at 1.5 hours), dropping temperature is controlled at 80 DEG C；
(3) drip rear keeping temperature to continue to react 2 hours, then add 30 kilograms of diallylamine, keeping temperature
Continue to react 2 hours, add the remaining deionized water and be diluted, after stirring, produce reactive dye it is positive from
Subtype aldehyde-free colour stabilizer.
By above-described embodiment one to the six directions into color fixing agent handle respectively reactive scarlet 3G dyeing after bafta, using leaching
Gu technique, color fixing agent consumption is 2% (o.w.f), pH is 6~7, and temperature is 60 DEG C, and the time is 30min, bath raio 1:12.Bafta
Main performance index after fixation is as shown in table 1.
Main performance index of the bafta of table 1 after the fixation treatment of above-described embodiment one to six
Remarks：
1. crock fastness method of testing presses GB/T3920-2008《Textile color stability tests colour fastness to rubbing》Method is surveyed
It is fixed；
2. soaping fastness method of testing presses GB/T3921-2008《Textile color stability tests color fastness to washing》Method is surveyed
It is fixed；
3. sweat leaching fastness method of testing presses GB/T5713-1997《Textile color stability tests color fastness to water》Method is surveyed
It is fixed.
4. color fixing agent G is the acrylonitrile-chlorinated ammonium color fixing agent of poly dimethyl diene, produced by Fujian Qingyuan Technology Co., Ltd., it is dense
Spend for 40%.
The present invention is by introducing tertiary amino, ester group isoreactivity group in color fixing agent structure, and with cationic properties, can
On reactive group, cellulosic molecule with dye molecule hydroxyl crosslinking, formed height diversification interconnected system, make dyestuff with
It is more firm that fiber is combined, so as to significantly improve the dry fastness, fastness to wet rubbing and color fastness to washing of reactive dye,
And do not influence the coloured light and feel of product.Make prepared fixation agent molecule that network structure is presented by crosslinking, film forming is strong.
After drying processing, soft, tough and tensile film is formed in fabric face.Prepared color fixing agent has dyefastness high, can improve
Dry and wet fastness, Washing, formaldehydeless pollution effectively reduce fabric formaldehyde content, lift the quality of fabric, environmental protection, dirt
Dye is small, with wide market prospects.
Described above, only using the embodiment of this origination techniques content, any those skilled in the art use this wound
Make done modifications and changes, all belong to the scope of the claims of this creation opinion, and be not limited to those disclosed embodiments.
Claims (1)
1. a kind of preparation method of reactive dye cationic formaldehyde-free fixing agent, it is characterised in that comprise the following steps：
（1）55~60 parts by weight dimethyl diallyl ammonium chlorides are added into reactor, stirring are opened, and begin to warm up liter
Temperature；
（2）When temperature rises to 60~90 DEG C, it is added dropwise simultaneously from two head tanks, 5.2~10 weight is added dropwise in the first head tank
Part tertiary-amino-containing monomer, the initiator that the mass percent concentration that 0.2~0.3 parts by weight are added dropwise in the second head tank is 1~10%
Solution, time for adding control was at 0.5~3 hour, and dropping temperature is controlled at 65~95 DEG C；
（3）Drip rear keeping temperature to continue to react 1~3 hour, then add 2.6~5 parts by weight of crosslinking agent, keeping temperature after
Continuous reaction 0.5~3 hour, adds deionized water and is diluted, after stirring, produce reactive dye cationic without aldehyde
Color fixing agent；
The tertiary-amino-containing monomer is dimethylaminoethyl acrylate, dimethylaminoethyl methacrylate, acrylic acid lignocaine third
In ester, dimethylaminoethyl methacrylate, dimethylaminoethyl propyl ester and methacrylic acid lignocaine propyl ester
Any one is two or more with any mixture than mixing；
The crosslinking agent is any one in diallylamine, triallylamine, N- amides or two or more
With any mixture than mixing；
The initiator is any one in ammonium persulfate, sodium peroxydisulfate or potassium peroxydisulfate or two or more with any ratio mixing
Mixture.
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| CN105175631B (en) * | 2013-12-27 | 2017-08-25 | 石狮市清源精细化工有限公司 | A kind of preparation method of reactive dye cationic formaldehyde-free fixing agent |
| CN105507013A (en) * | 2015-11-24 | 2016-04-20 | 福建隆上超纤有限公司 | An after-finishing process for superfine fiber synthetic leather |
| CN108179642B (en) * | 2016-05-20 | 2020-11-13 | 南通市武鑫化工有限公司 | Preparation method of color fixing agent for reactive dye dyeing |
| CN105908543A (en) * | 2016-06-07 | 2016-08-31 | 苏州联胜化学有限公司 | Environment-friendly chlorine-resistant fastness improving agent for cotton and preparation method of fastness improving agent |
| CN106555347A (en) * | 2016-11-28 | 2017-04-05 | 佛山市飞时达新材料科技有限公司 | A kind of water-soluble dye color fixing agent containing ibuprofen and its preparation, using method |
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| CN108659170A (en) * | 2018-07-05 | 2018-10-16 | 陈国宝 | A kind of printing and dyeing color fixing agent and preparation method thereof |
| CN108824035A (en) * | 2018-07-05 | 2018-11-16 | 陈国宝 | A kind of fabrics printing and dyeing color fixing agent and preparation method thereof |
| CN109096437A (en) * | 2018-07-07 | 2018-12-28 | 曾文华 | A kind of acid dyes aldehyde-free colour stabilizer and preparation method thereof |
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| CN110331605B (en) * | 2019-07-19 | 2021-10-08 | 绍兴中纺化工有限公司 | Natural dye color fixing agent and preparation method thereof |
| CN110591011B (en) * | 2019-09-09 | 2021-09-28 | 张家港市德宝化工有限公司 | Process method for preparing color fixing agent by using special acrylate wastewater |
| CN112376301A (en) * | 2020-11-16 | 2021-02-19 | 浙江大川新材料股份有限公司 | Formaldehyde-free color fixing agent and preparation method and application thereof |
| CN115726203A (en) * | 2021-08-31 | 2023-03-03 | 传清化工(广东)有限公司 | Polyester cotton high-fastness fixing agent and preparation method thereof |
| CN115584649B (en) * | 2021-12-29 | 2023-11-28 | 清远市宏图助剂有限公司 | Cationic polymer formaldehyde-free color fixing agent, preparation method and application thereof |
| CN115094654B (en) * | 2022-08-23 | 2022-12-20 | 江苏富淼科技股份有限公司 | Polymer color fixing agent and preparation method thereof |
| CN115748271A (en) * | 2022-10-26 | 2023-03-07 | 浙江海联新材料科技有限公司 | Ternary polymerization efficient formaldehyde-free color fixing agent for reactive dye and preparation method thereof |
| CN116463868A (en) * | 2023-04-11 | 2023-07-21 | 宁波澳翔精细化工有限公司 | Aldehyde-free color fixing agent and preparation method thereof |
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