CN105908542B - A kind of color fixing agent of ramie fabric liquefied ammonia solvent dyeing and preparation method and application method - Google Patents
A kind of color fixing agent of ramie fabric liquefied ammonia solvent dyeing and preparation method and application method Download PDFInfo
- Publication number
- CN105908542B CN105908542B CN201610325118.0A CN201610325118A CN105908542B CN 105908542 B CN105908542 B CN 105908542B CN 201610325118 A CN201610325118 A CN 201610325118A CN 105908542 B CN105908542 B CN 105908542B
- Authority
- CN
- China
- Prior art keywords
- fixing agent
- color fixing
- liquefied ammonia
- ramie fabric
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 0 CC(C)C(C)C(N**(C)C)=O Chemical compound CC(C)C(C)C(N**(C)C)=O 0.000 description 2
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
- D06P5/08—After-treatment with organic compounds macromolecular
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/38—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using reactive dyes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/81—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dyes dissolved in inorganic solvents
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/008—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated using reactive dyes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/66—Natural or regenerated cellulose using reactive dyes
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Coloring (AREA)
Abstract
The present invention relates to a kind of color fixing agent of ramie fabric liquefied ammonia solvent dyeing and preparation method and application method, belong to technical field of textile chemistry.N NMAs addition dimethylamine is first added hydrochloric acid by the present invention, obtains N (dimethylammonium hydrochloride) Methacrylamide；The allyl polyethenoxy ether monomer that the degree of polymerization is 45 is dissolved in appropriate deionized water again, allyl polyethenoxy ether solution is made；Then N (dimethylammonium hydrochloride) Methacrylamides and allyl polyethenoxy ether solution are added drop-wise in the four-hole boiling flask equipped with a certain amount of deionized water simultaneously with these three solution of ammonium persulfate initiator solution, time for adding control is 2~3 hours, by temperature control in 75~80 DEG C of stirring reactions；After being added dropwise, 3~4 hours are incubated；Obtain the color fixing agent.The weight average molecular weight of the color fixing agent is 3000~10000.Color fixing agent produced by the present invention is used in ramie fabric liquefied ammonia solvent dyeing, the washing fastness of ramie fabric can be significantly improved.
Description
Technical field
The invention belongs to technical field of textile chemistry, and in particular to a kind of color fixing agent of ramie fabric liquefied ammonia solvent dyeing and
Its preparation method and application process.
Background technology
Textile industry is the conventional column industry of Chinese national economy and important people's livelihood industry, and international competitive advantage
Obvious industry, ramee are one of primary raw materials of weaving face fabric, and critical role is occupied in weaving face fabric.China is generation
, mainly there are ramie, sisal hemp, flax and yellow mestha etc. in one of most abundant country of hemp resource in boundary, wherein, ramie is grown with it
The advantages that speed is fast, yield is high, easy survival is planted extensively in China.The fabric that ramee is made into has ventilative, moisture absorbing and sweat releasing
The advantages that, it is preferable summer high-grade clothing fabric.But the characteristics such as crystallinity and degree of orientation height due to ramee, cause it
Phenomena such as easily being decolourized after dyeing, washing fastness is low.The presence of this problem prevents its advantage from fully bringing into play,
So as to significantly limit its use.
In recent years, China's textile industry ecological circulation economic development contradiction, the height of water resource is relied on and
Environmental problem caused by maximum discharge seriously governs the sustainable development of the sector.According to statistics, China's textile printing and dyeing industry year is consumed
1,700,000,000 tons of water, disposal of pollutants is up to 1,600,000,000 tons.Compared with foreign countries, the water consumption of China's textile printing and dyeing industry is external 2-3
Times, energy consumption is external 3-5 times.Because traditional colouring method is using water as medium, cleaned after dyeing with water, water consumption is big, makes
Chemical assistant is more, administers difficult.Few water or non-aqueous dyeing turn into the side that traditional dyeing is transformed as a key areas
To.Therefore, dyeing of the applicant to ramee in liquefied ammonia solvent conducts extensive research.As a result find, ramee
After being dyed in liquefied ammonia solvent, fabric is it sometimes appear that problems such as washing fastness are low, and in order to solve this problem, prepared by applicant
The color fixing agent being used in this dyeing system.
At present, commercially, the patent in color fixing agent field is relatively more, for example, Application No. 201010013592.2 is special
Profit application discloses a kind of cation type reactive polyurethane coloring stabilizer and preparation method thereof, and the color fixing agent is not belonging to polyphosphazene polymer
Compound, mainly for the fixation of the fabric such as deep-colour fabric and silk, wool, products obtained therefrom is emulsion, it is clear that emulsion is to mix
It is added in liquefied ammonia dicyandiamide solution, because both can not dissolve each other at low temperature.In addition, Application No. 201410289992.4 is special
Profit application also discloses that a kind of color fixing process of response type cationic fixing agent in cotton fabrics dyed with reactive dyes, the color fixing agent
In cation group can be combined with the anionic group in anionic dyes structure with ionic bond, epoxy radicals can be with cotton
Hydroxyl in fabric crosslinks reaction, and color fixing agent " bridge formation " between dyestuff and fiber forms compound, forms cross-linking system,
Prevent dyestuff from being come off from fiber, improve the dyefastness of dyestuff；According to this reaction mechanism, in the lower temperature of liquefied ammonia system
Under, epoxy radicals can not crosslink reaction with the hydroxyl in ramie fabric, therefore the color fixing agent cannot act as the fixation of liquefied ammonia system
Agent.
Domestic and international market is to ecological textile and the requirement more and more higher of environmental protection, the need of few water or waterless staining technique
Ask increasing, environment-friend auxiliaries turn into the product that domestic and international textile auxiliary company competitively develops.Find and develop new dyeing
The environment-friend auxiliaries of technology, turn into field of printing and dyeing urgent problem to be solved.
The content of the invention
The present invention is directed to the problem of pointed in background technology and the shortcomings of the prior art, of the invention first mesh
Be a kind of color fixing agent for ramie fabric liquefied ammonia solvent dyeing is provided, the color fixing agent is a kind of high molecular polymer,
With more polyoxyethylene group, the group can be combined with amino molecule in a manner of hydrogen bond, have preferable ammonia dissolubility.Ramie
Fabric is in liquefied ammonia solvent dyeing, and after adding this color fixing agent, the washing fastness of fabric significantly improves.
In addition, present invention also offers a kind of preparation side of the color fixing agent of ramie fabric liquefied ammonia solvent dyeing described above
Method and application process.
In order to realize above-mentioned first purpose of the present invention, inventor passes through substantial amounts of experimental study, have developed one kind
The color fixing agent of ramie fabric liquefied ammonia solvent dyeing, the structural formula of the color fixing agent are as follows：
Wherein, a is that 3~6, b is 2~5, and the weight average molecular weight of the color fixing agent is 3000~10000.
Another object of the present invention is to provide a kind of system of the color fixing agent of ramie fabric liquefied ammonia solvent dyeing described above
Preparation Method, methods described comprise the following steps：
The first step：The preparation of N- (dimethylammonium hydrochloride) Methacrylamide：N hydroxymethyl acrylamide is added three mouthfuls
Flask, is warming up to 50 DEG C by temperature, adds dimethylamine stirring reaction 4 hours, then adds hydrochloric acid reaction 1 hour, obtains N- (two
Ammonium carbamate hydrochlorate) Methacrylamide, wherein, N hydroxymethyl acrylamide, dimethylamine, the mol ratio of hydrochloric acid are 1：1~1.5：1
~1.5；
Second step：The preparation of allyl polyethenoxy ether solution：By the allyl polyethenoxy ether monomer that the degree of polymerization is 45
It is dissolved in appropriate deionized water, allyl polyethenoxy ether solution is made；
3rd step：The preparation of color fixing agent：By (dimethylammonium hydrochloride) Methacrylamides of N- made from the above-mentioned first step and
These three solution of allyl polyethenoxy ether solution and ammonium persulfate initiator solution made from second step are added drop-wise to and are equipped with simultaneously
In the four-hole boiling flask of a certain amount of deionized water, rate of addition is controlled with constant flow pump, time for adding control is 2~3 hours, in flask
A small amount of deionized water is added, by temperature control in 75~80 DEG C of stirring reactions；After being added dropwise to complete, 3~4 hours are incubated, is gathered
(N- (dimethylammonium hydrochloride) Methacrylamide)-polyallyl APEO, i.e., described color fixing agent, gel permeation chromatography are surveyed
Its molecular weight is tried, its weight average molecular weight reaches 3000~10000, and this color fixing agent is freezed, and dries, standby, wherein, N- (diformazans
Ammonium salt hydrochlorate) Methacrylamide, allyl polyethenoxy ether monomer and ammonium persulfate initiator mol ratio be 1：0.8~1：
0.1~0.5.
Further, the concentration of hydrochloric acid described in step 1 is 15~20% in above-mentioned technical proposal.
Further, in above-mentioned technical proposal N hydroxymethyl acrylamide, dimethylamine, hydrochloric acid described in step 1 mol ratio
Preferably 1：1：1.
Further, N- described in step 3 (dimethylammonium hydrochloride) Methacrylamide, pi-allyl in above-mentioned technical proposal
The mol ratio of polyoxyethylene ether monomer and ammonium persulfate initiator is preferably 1：1：0.3.
The chemical reaction that the preparation method of the color fixing agent of the above-mentioned ramie fabric liquefied ammonia solvent dyeing of the present invention is related to
It is as follows：
The chemical reaction that the first step is related to：
The chemical reaction that second step is related to：
The a further object of the present invention is to provide a kind of color fixing agent of ramie fabric liquefied ammonia solvent dyeing obtained above
Application process, concretely comprise the following steps：
The first step：The ramie fabric of certain mass is chosen, ramie fabric is immersed in the liquefied ammonia dye liquor dissolved with reactive dye
In dyed, wherein, dye dosage >=5% (o.m.f), bath raio 1：30, under conditions of dyeing time >=25 second, contaminated
Color thing, product dyed thereby is dried, standby；
Second step：The color fixing agent of certain mass is dissolved in liquid ammonia solution, consolidated what the product dyed thereby immersion of the first step prepared
In toner liquid ammonia solution, fixation time >=25 second, color fixing agent dosage is the 1~3% of dye dosage, drying is taken out, after obtaining fixation
Product dyed thereby.
Further, the 3rd step is also included in above-mentioned technical proposal：Soap, be in bath raio by the fixation product dyed thereby after drying
1：50, concentration is that soap 15 min in 100 DEG C in 2 g/L non-ionic detergent agent solution, and drying is standby；Then contaminated
The measure of color thing washing color fastness：This product dyed thereby is carried out to the measure of washing fastness, method for making sample is resistance to by ISO105-C06
Prepared by Washing method, method of testing is determined by GB/T251-2008 grey scale for assessing staining of colour method, test result
For：4~5.
The preparation reaction principle of the present invention：In the preparation process of Inventive polymers cationic fixing agent, first by N-
NMA carries out cationization processing, obtains N- (dimethylammonium hydrochloride) Methacrylamide cationic monomer；So
Afterwards, by N- (dimethylammonium hydrochloride) Methacrylamide cationic monomers and allyl polyethenoxy ether monomer（The degree of polymerization is 45）
Carry out Raolical polymerizable, obtain poly- (N- (dimethylammonium hydrochloride) Methacrylamide)-polyallyl APEO.
The high molecular polymer color fixing agent of the present invention has more ethoxy based structures, and ethyoxyl can utilize with amino molecule
Hydrogen bond action combines well, and therefore, this color fixing agent is to dissolve well in liquefied ammonia.It is fine as ramie in liquefied ammonia system
The color fixing agent of dimension, its dye fixative theory can be analyzed as follows：
(1) ethyoxyl of this color fixing agent can also be combined well with reactive dyestuff molecule using hydrogen bond action, in addition,
The cation group of this color fixing agent is combined with the anionic group of reactive dye with ionic bond, so as to fixation agent molecule and dyestuff
Molecule, cellulosic molecule are cross-linked with each other, so as to reduce the ammonia dissolubility of dyestuff；
（2）This color fixing agent is high molecular polymer, in the surface filming of ramee, can make the reduction that comes off of dyestuff.
Compared with prior art, the present invention has following beneficial effect：
（1）Raw material sources of the present invention are extensive, and cost is low, and obtained cationic fixing agent belongs to high molecular polymer, molecule
Measure larger, weight average molecular weight reaches 3000~10000, can preferably be dissolved in liquefied ammonia solvent；Polymer sun prepared by the present invention from
For sub- color fixing agent without the harmful substance such as formaldehyde, total alkali content is low, and to environment without any pollution, green, preparation process is simple, in
Between product without separation, final finishing on ramie fabric influences small, is easy to production and quality control；
（2）Polymer cation color fixing agent produced by the present invention is used for ramie fabric after liquefied ammonia solvent dyeing, ramie
The washing fastness of linen significantly increases, and shows that the fixation of ramie fabric achieves the goal, polymer cation of the invention is consolidated
Toner is advantageous to the dyeing of ramie and the exploitation of Printing, and the successful implementation for anhydrous dyeing and finishing technique provides important leverage；
（3）The present invention solves the problems, such as that production process energy consumption is big in existing ramie fabric dyeing, water pollution is serious, carries
High washing fastness of the reactive dye in liquefied ammonia dyeing, solve the problems such as fixation difference in ramie fabric dyeing course, have
Have dyeing processing step it is few, dyeing time is short, dyestuff reusable edible after dye, the advantages that reducing environmental pollution, can be achieved ramie
Non-aqueous dyeing requirement during textile dyeing.
Embodiment
Form is described in further detail again to the above of the present invention by the following examples, but should not manage this
The scope solved as the above-mentioned theme of the present invention is only limitted to following embodiment, and all technologies for being realized based on the above of the present invention are equal
Belong to the scope of the present invention.
Embodiment 1：
A kind of color fixing agent of ramie fabric liquefied ammonia solvent dyeing of the present embodiment, the color fixing agent are prepared with the following method
Form, comprise the following steps：
The first step：The preparation of N- (dimethylammonium hydrochloride) Methacrylamide：0.1mol N hydroxymethyl acrylamides are added
Enter three-necked flask, temperature is warming up to 50 DEG C, adds 0.1mol dimethylamine stirring reaction 4 hours, then adds 0.1mol concentration
For 18% hydrochloric acid reaction 1 hour, N- (dimethylammonium hydrochloride) Methacrylamide is obtained, IR, HNMR prove product structure such as
Under.
Second step：The preparation of allyl polyethenoxy ether solution：By the allyl polyethenoxy that the 0.1mol degree of polymerization is 45
Ether monomer is dissolved in 20 grams of deionized water, and allyl polyethenoxy ether solution is made.
3rd step：The preparation of color fixing agent：By (dimethylammonium hydrochloride) Methacrylamides of N- made from the above-mentioned first step and
Allyl polyethenoxy ether solution and ammonium persulfate solution made from second step（0.01mol ammonium persulfates be dissolved in 20 grams go from
Sub- water is made）These three solution are added drop-wise in the four-hole boiling flask equipped with a certain amount of deionized water simultaneously, are controlled and are added dropwise with constant flow pump
Speed, time for adding control are 2~3 hours, and 50mL deionized waters are added in flask, and temperature control is anti-in 75~80 DEG C of stirrings
Should；After being added dropwise to complete, 3~4 hours are incubated, obtains poly- (N- (dimethylammonium hydrochloride) Methacrylamide)-polyallyl polyoxy
Vinethene, IR, HNMR, GPC prove that product structure is as follows, and the weight average molecular weight that the product is determined by GPC is 4900.By product
Freeze-drying, grind into powder are standby.
The application of the present embodiment color fixing agent described above as follows, comprises the following steps：
The first step：5g ramie fabrics are weighed, ramie fabric is immersed in the liquefied ammonia dye liquor dissolved with reactive dye Reactive Red 2
Dyed, wherein, dye dosage 5% (o.m.f), bath raio 1：30, dyeing time obtains product dyed thereby under conditions of 25 seconds, will
Product dyed thereby is dried, standby.
Second step：The color fixing agent of certain mass is dissolved in liquid ammonia solution, consolidated what the product dyed thereby immersion of the first step prepared
In the liquid ammonia solution of toner, 25 seconds fixation time, color fixing agent dosage is the 1% of dye dosage, drying is taken out, after obtaining fixation
Product dyed thereby.
3rd step：Soap：By the fixation product dyed thereby after drying bath raio be 1：50, concentration is 2 g/L non-ionic detergent
In agent solution, soap 15 min in 100 DEG C, is dried for standby；Then the measure of product dyed thereby washing color fastness is carried out：This is contaminated
Color thing carries out the measure of washing fastness, and method for making sample is prepared by ISO105-C06 washing color fastness method, and method of testing is pressed
GB/T251-2008 grey scale for assessing staining of colour method determines, and test result is：4~5.
Embodiment 2：
A kind of polymer cation color fixing agent for ramie fabric of the present embodiment, the polymer cation color fixing agent
It is prepared, comprises the following steps with the following method：
The first step：The preparation of N- (dimethylammonium hydrochloride) Methacrylamide：0.1mol N hydroxymethyl acrylamides are added
Enter three-necked flask, temperature is warming up to 50 DEG C, adds 0.15mol dimethylamine stirring reaction 4 hours, it is dense then to add 0.1mol
The hydrochloric acid reaction 1 hour for 18% is spent, obtains N- (dimethylammonium hydrochloride) Methacrylamide, IR, HNMR prove product structure such as
Under.
Second step：The preparation of allyl polyethenoxy ether solution：By the allyl polyethenoxy that the 0.08mol degree of polymerization is 45
Ether monomer is dissolved in 20 grams of deionized water, and allyl polyethenoxy ether solution is made.
3rd step：The preparation of color fixing agent：By (dimethylammonium hydrochloride) Methacrylamides of N- made from the above-mentioned first step and
Allyl polyethenoxy ether solution and ammonium persulfate solution made from second step（0.02mol ammonium persulfates be dissolved in 20 grams go from
Sub- water is made）These three solution are added drop-wise in the four-hole boiling flask equipped with a certain amount of deionized water to be controlled with constant flow pump simultaneously is added dropwise speed
Degree, time for adding control are 2~3 hours, and 50mL deionized waters are added in flask, and temperature control is anti-in 75~80 DEG C of stirrings
Should；After being added dropwise to complete, 3~4 hours are incubated, obtains poly- (N- (dimethylammonium hydrochloride) Methacrylamide)-polyallyl polyoxy
Vinethene, IR, HNMR, GPC prove that product structure is as follows, and the weight average molecular weight that the product is determined by GPC is 4500.By product
Freeze-drying, grind into powder are standby.
The application of the present embodiment color fixing agent described above as follows, comprises the following steps：
The first step：5g ramie fabrics are weighed, ramie fabric is immersed in the liquefied ammonia dye liquor dissolved with reactive dye Reactive Red 2
Dyed, wherein, dye dosage 5% (o.m.f), bath raio 1：30, dyeing time obtains product dyed thereby under conditions of 25 seconds, will
Product dyed thereby is dried, standby.
Second step：The color fixing agent of certain mass is dissolved in liquid ammonia solution, consolidated what the product dyed thereby immersion of the first step prepared
In the liquid ammonia solution of toner, 25 seconds fixation time, color fixing agent dosage is the 2% of dye dosage, drying is taken out, after obtaining fixation
Product dyed thereby.
3rd step：Soap：By the fixation product dyed thereby after drying bath raio be 1：50, concentration is 2 g/L non-ionic detergent
In agent solution, soap 15 min in 100 DEG C, is dried for standby；Then the measure of product dyed thereby washing color fastness is carried out：This is contaminated
Color thing carries out the measure of washing fastness, and method for making sample is prepared by ISO105-C06 washing color fastness method, and method of testing is pressed
GB/T251-2008 grey scale for assessing staining of colour method determines, and test result is：4~5.
Embodiment 3：
A kind of polymer cation color fixing agent for ramie fabric of the present embodiment, the polymer cation color fixing agent
It is prepared, comprises the following steps with the following method：
The first step：The preparation of N- (dimethylammonium hydrochloride) Methacrylamide：0.1mol N hydroxymethyl acrylamides are added
Enter three-necked flask, temperature is warming up to 50 DEG C, adds 0.1mol dimethylamine stirring reaction 4 hours, it is dense then to add 0.15mol
The hydrochloric acid reaction 1 hour for 18% is spent, obtains N- (dimethylammonium hydrochloride) Methacrylamide, IR, HNMR prove product structure such as
Under.
Second step：The preparation of allyl polyethenoxy ether solution：By the allyl polyethenoxy that the 0.08mol degree of polymerization is 45
Ether monomer is dissolved in 20 grams of deionized water, and allyl polyethenoxy ether solution is made.
3rd step：The preparation of color fixing agent：By (dimethylammonium hydrochloride) Methacrylamides of N- made from the above-mentioned first step and
Allyl polyethenoxy ether solution and ammonium persulfate solution made from second step（0.03mol ammonium persulfates be dissolved in 20 grams go from
Sub- water is made）These three solution are added drop-wise in the four-hole boiling flask equipped with a certain amount of deionized water simultaneously, are controlled and are added dropwise with constant flow pump
Speed, time for adding control are 2~3 hours, and 50mL deionized waters are added in flask, and temperature control is anti-in 75~80 DEG C of stirrings
Should；After being added dropwise to complete, 3~4 hours are incubated, obtains poly- (N- (dimethylammonium hydrochloride) Methacrylamide)-polyallyl polyoxy
Vinethene, IR, HNMR, GPC prove that product structure is as follows, and the weight average molecular weight that the product is determined by GPC is 5900.By product
Freeze-drying, grind into powder are standby.
The application of the present embodiment color fixing agent described above as follows, comprises the following steps：
The first step：5g ramie fabrics are weighed, ramie fabric is immersed in the liquefied ammonia dye liquor dissolved with reactive dye Reactive Red 2
Dyed, wherein, dye dosage 5% (o.m.f), bath raio 1：30, dyeing time obtains product dyed thereby under conditions of 30 seconds, will
Product dyed thereby is dried, standby.
Second step：The color fixing agent of certain mass is dissolved in liquid ammonia solution, consolidated what the product dyed thereby immersion of the first step prepared
In the liquid ammonia solution of toner, 25 seconds fixation time, color fixing agent dosage is the 3% of dye dosage, drying is taken out, after obtaining fixation
Product dyed thereby.
3rd step：Soap：By the fixation product dyed thereby after drying bath raio be 1：50, concentration is 2 g/L non-ionic detergent
In agent solution, soap 15 min in 100 DEG C, is dried for standby；Then the measure of product dyed thereby washing color fastness is carried out：This is contaminated
Color thing carries out the measure of washing fastness, and method for making sample is prepared by ISO105-C06 washing color fastness method, and method of testing is pressed
GB/T251-2008 grey scale for assessing staining of colour method determines, and test result is：5.
Embodiment 4：
A kind of polymer cation color fixing agent for ramie fabric of the present embodiment, the polymer cation color fixing agent
It is prepared, comprises the following steps with the following method：
The first step：The preparation of N- (dimethylammonium hydrochloride) Methacrylamide：0.1mol N hydroxymethyl acrylamides are added
Enter three-necked flask, temperature is warming up to 50 DEG C, adds 0.15mol dimethylamine stirring reaction 4 hours, it is dense then to add 0.15mol
The hydrochloric acid reaction 1 hour for 18% is spent, obtains N- (dimethylammonium hydrochloride) Methacrylamide, IR, HNMR prove product structure such as
Under.
Second step：The preparation of allyl polyethenoxy ether solution：By the allyl polyethenoxy that the 0.1mol degree of polymerization is 45
Ether monomer is dissolved in 20 grams of deionized water, and allyl polyethenoxy ether solution is made.
3rd step：The preparation of color fixing agent：By (dimethylammonium hydrochloride) Methacrylamides of N- made from the above-mentioned first step and
Allyl polyethenoxy ether solution and ammonium persulfate solution made from second step（0.05mol ammonium persulfates be dissolved in 20 grams go from
Sub- water is made）These three solution are added drop-wise in the four-hole boiling flask equipped with a certain amount of deionized water simultaneously, are controlled and are added dropwise with constant flow pump
Speed, time for adding control are 2~3 hours, and 50mL deionized waters are added in flask, and temperature control is anti-in 75~80 DEG C of stirrings
Should；After being added dropwise to complete, 3~4 hours are incubated, obtains poly- (N- (dimethylammonium hydrochloride) Methacrylamide)-polyallyl polyoxy
Vinethene, IR, HNMR, GPC prove that product structure is as follows, and the weight average molecular weight that the product is determined by GPC is 3900.By product
Freeze-drying, grind into powder are standby.
The application of the present embodiment color fixing agent described above as follows, comprises the following steps：
The first step：5g ramie fabrics are weighed, ramie fabric is immersed in the liquefied ammonia dye liquor dissolved with reactive dye Reactive Red 2
Dyed, wherein, dye dosage 5% (o.m.f), bath raio 1：30, dyeing time obtains product dyed thereby under conditions of 25 seconds, will
Product dyed thereby is dried, standby.
Second step：The color fixing agent of certain mass is dissolved in liquid ammonia solution, consolidated what the product dyed thereby immersion of the first step prepared
In the liquid ammonia solution of toner, 25 seconds fixation time, color fixing agent dosage is the 2% of dye dosage, drying is taken out, after obtaining fixation
Product dyed thereby.
3rd step：Soap：By the fixation product dyed thereby after drying bath raio be 1：50, concentration is 2 g/L non-ionic detergent
In agent solution, soap 15 min in 100 DEG C, is dried for standby；Then the measure of product dyed thereby washing color fastness is carried out：This is contaminated
Color thing carries out the measure of washing fastness, and method for making sample is prepared by ISO105-C06 washing color fastness method, and method of testing is pressed
GB/T251-2008 grey scale for assessing staining of colour method determines, and test result is：5.
Embodiment 5：
A kind of polymer cation color fixing agent for ramie fabric of the present embodiment, the polymer cation color fixing agent
It is prepared, comprises the following steps with the following method：
The first step：The preparation of N- (dimethylammonium hydrochloride) Methacrylamide：0.1mol N hydroxymethyl acrylamides are added
Enter three-necked flask, temperature is warming up to 50 DEG C, adds 0.1mol dimethylamine stirring reaction 4 hours, then adds 0.1mol concentration
For 18% hydrochloric acid reaction 1 hour, N- (dimethylammonium hydrochloride) Methacrylamide is obtained, IR, HNMR prove product structure such as
Under.
Second step：The preparation of allyl polyethenoxy ether solution：By the allyl polyethenoxy that the 0.1mol degree of polymerization is 45
Ether monomer is dissolved in 20 grams of deionized water, and allyl polyethenoxy ether solution is made.
3rd step：The preparation of color fixing agent：By (dimethylammonium hydrochloride) Methacrylamides of N- made from the above-mentioned first step and
Allyl polyethenoxy ether solution and ammonium persulfate solution made from second step（0.04mol ammonium persulfates be dissolved in 20 grams go from
Sub- water is made）These three solution are added drop-wise in the four-hole boiling flask equipped with a certain amount of deionized water simultaneously, are controlled and are added dropwise with constant flow pump
Speed, time for adding control are 2~3 hours, and 50mL deionized waters are added in flask, and temperature control is anti-in 75~80 DEG C of stirrings
Should；After being added dropwise to complete, 3~4 hours are incubated, obtains poly- (N- (dimethylammonium hydrochloride) Methacrylamide)-polyallyl polyoxy
Vinethene, IR, HNMR, GPC prove that product structure is as follows, and the weight average molecular weight that the product is determined by GPC is 7500.By product
Freeze-drying, grind into powder are standby.
The application of the present embodiment color fixing agent described above as follows, comprises the following steps：
The first step：5g ramie fabrics are weighed, ramie fabric is immersed in the liquefied ammonia dye liquor dissolved with reactive dye Reactive Red 2
Dyed, wherein, dye dosage 5% (o.m.f), bath raio 1：30, dyeing time obtains product dyed thereby under conditions of 25 seconds, will
Product dyed thereby is dried, standby.
Second step：The color fixing agent of certain mass is dissolved in liquid ammonia solution, consolidated what the product dyed thereby immersion of the first step prepared
In the liquid ammonia solution of toner, 25 seconds fixation time, color fixing agent dosage is the 2% of dye dosage, drying is taken out, after obtaining fixation
Product dyed thereby.
3rd step：Soap：By the fixation product dyed thereby after drying bath raio be 1：50, concentration is 2 g/L non-ionic detergent
In agent solution, soap 15 min in 100 DEG C, is dried for standby；Then the measure of product dyed thereby washing color fastness is carried out：This is contaminated
Color thing carries out the measure of washing fastness, and method for making sample is prepared by ISO105-C06 washing color fastness method, and method of testing is pressed
GB/T251-2008 grey scale for assessing staining of colour method determines, and test result is：5.
Claims (7)
1. a kind of color fixing agent of ramie fabric liquefied ammonia solvent dyeing, the structural formula of the color fixing agent are as follows：
Wherein, a is that 3~6, b is 2~5, and the weight average molecular weight of the color fixing agent is 3000~10000.
A kind of 2. preparation method of the color fixing agent of ramie fabric liquefied ammonia solvent dyeing, for preparing the fixation described in claim 1
Agent, it is characterised in that：Methods described comprises the following steps：
The first step：The preparation of N- (dimethylammonium hydrochloride) Methacrylamide：N hydroxymethyl acrylamide is added into three-necked flask,
Temperature is warming up to 50 DEG C, adds dimethylamine stirring reaction 4 hours, then adds hydrochloric acid reaction 1 hour, obtains N- (dimethylammoniums
Hydrochloride) Methacrylamide, wherein, N hydroxymethyl acrylamide, dimethylamine, hydrochloric acid mol ratio for the ︰ 1 of 1 ︰ 1~1.5~
1.5；
Second step：The preparation of allyl polyethenoxy ether solution：The allyl polyethenoxy ether monomer that the degree of polymerization is 45 is dissolved
In appropriate deionized water, allyl polyethenoxy ether solution is made；
3rd step：The preparation of color fixing agent：By N- made from the above-mentioned first step (dimethylammonium hydrochloride) Methacrylamide and second
Allyl polyethenoxy ether solution made from step is added drop-wise to equipped with certain simultaneously with these three solution of ammonium persulfate initiator solution
In the four-hole boiling flask for measuring deionized water, rate of addition is controlled with constant flow pump, time for adding control is 2~3 hours, is added in flask
A small amount of deionized water, by temperature control in 75~80 DEG C of stirring reactions；After being added dropwise to complete, 3~4 hours are incubated, obtains poly- (N-
(dimethylammonium hydrochloride) Methacrylamide)-polyallyl APEO, i.e., described color fixing agent, gel permeation chromatography test
Its molecular weight, its weight average molecular weight reach 3000~10000, and this color fixing agent is freezed, and dry, standby, wherein, N- (dimethylammoniums
Hydrochloride) mol ratio of Methacrylamide, allyl polyethenoxy ether monomer and ammonium persulfate initiator is the ︰ of 1 ︰ 0.8~1
0.1~0.5.
3. the preparation method of the color fixing agent of ramie fabric liquefied ammonia solvent dyeing according to claim 2, it is characterised in that：Step
The concentration of the rapid hydrochloric acid is 15~20%.
4. the preparation method of the color fixing agent of ramie fabric liquefied ammonia solvent dyeing according to claim 2, it is characterised in that：Step
A rapid N hydroxymethyl acrylamide, dimethylamine, the mol ratio of hydrochloric acid are preferably the ︰ 1 of 1 ︰ 1.
5. the preparation method of the color fixing agent of ramie fabric liquefied ammonia solvent dyeing according to claim 2, it is characterised in that：Step
Rapid three N- (dimethylammonium hydrochloride) Methacrylamide, allyl polyethenoxy ether monomer and ammonium persulfate initiator are rubbed
You are than the ︰ 0.3 of preferably 1 ︰ 1.
A kind of 6. application process of the color fixing agent of ramie fabric liquefied ammonia solvent dyeing, using described in claim 1 to 5 any one
Color fixing agent, it is characterised in that：Concretely comprise the following steps：
The first step：The ramie fabric of certain mass is chosen, ramie fabric is immersed in the liquefied ammonia dye liquor dissolved with reactive dye
Row dyeing, wherein, dye dosage >=5% (o.m.f), bath raio 1：30, under conditions of dyeing time >=25 second, dyed
Thing, product dyed thereby is dried, it is standby；
Second step：The color fixing agent of certain mass is dissolved in liquid ammonia solution, the product dyed thereby of the first step is immersed to the color fixing agent prepared
In liquid ammonia solution, fixation time >=25 second, color fixing agent dosage is the 1~3% of dye dosage, drying is taken out, after obtaining fixation
Product dyed thereby.
7. the application process of the color fixing agent of ramie fabric liquefied ammonia solvent dyeing according to claim 6, it is characterised in that：Also
Including the 3rd step：Soap, by the fixation product dyed thereby after drying bath raio be 1：50, concentration is 2g/L non-ionic detergent agent solution
In, it is standby in 100 DEG C of 15min that soap, drying；Then the measure of product dyed thereby washing color fastness is carried out：This product dyed thereby is carried out
The measure of washing fastness, method for making sample are prepared by ISO105-C06 washing color fastness method, and method of testing presses GB/T251-
2008 grey scale for assessing staining of colour methods determine, and test result is：4~5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610325118.0A CN105908542B (en) | 2016-05-17 | 2016-05-17 | A kind of color fixing agent of ramie fabric liquefied ammonia solvent dyeing and preparation method and application method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610325118.0A CN105908542B (en) | 2016-05-17 | 2016-05-17 | A kind of color fixing agent of ramie fabric liquefied ammonia solvent dyeing and preparation method and application method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105908542A CN105908542A (en) | 2016-08-31 |
| CN105908542B true CN105908542B (en) | 2017-12-08 |
Family
ID=56749275
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610325118.0A Active CN105908542B (en) | 2016-05-17 | 2016-05-17 | A kind of color fixing agent of ramie fabric liquefied ammonia solvent dyeing and preparation method and application method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105908542B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106436278B (en) * | 2016-10-11 | 2018-09-25 | 武汉纺织大学 | A kind of ammoniation modified method of ramee and its application process in liquefied ammonia solvent dyeing |
| CN106544905B (en) * | 2016-12-12 | 2018-11-02 | 江西德盛精细化学品有限公司 | A kind of preparation method of seamless underwear acidic color fixing agent and color fixing agent obtained |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2693731B1 (en) * | 1992-07-15 | 1994-10-21 | Centre Nat Rech Scient | Oxirane and dioxolane copolymers, their preparation process and ionically conductive materials containing them. |
| CN102127193B (en) * | 2011-01-30 | 2012-07-18 | 安徽大学 | Method for preparing cationic poly(urethane-dimethyldiallylammonium chloride) color fixing agent |
| CN103225218B (en) * | 2013-04-10 | 2016-04-20 | 武汉纺织大学 | A kind of liquefied ammonia colouring method of cellulose fibre |
| CN104099790B (en) * | 2014-07-09 | 2016-04-20 | 武汉纺织大学 | A kind of method utilizing liquefied ammonia eccysis fiber loose colour |
| CN105175672A (en) * | 2015-10-22 | 2015-12-23 | 上海上萃精细化工有限公司 | Anionic polyurethane color fixative and synthesis method thereof |
| CN105350329B (en) * | 2015-11-24 | 2017-07-07 | 武汉纺织大学 | A kind of polymer cation modifying agent for ramie fabric and preparation method and application method |
-
2016
- 2016-05-17 CN CN201610325118.0A patent/CN105908542B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN105908542A (en) | 2016-08-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106220785B (en) | A kind of preparation method and application of the reactivity polyquarternium-type without aldehyde fixation crosslinking agent | |
| CN105111363B (en) | A kind of function performed polymer and preparation method and application | |
| CN106436278B (en) | A kind of ammoniation modified method of ramee and its application process in liquefied ammonia solvent dyeing | |
| CN106436327B (en) | A kind of modified amido organic fluorinated silicone fat liquor increases deep finishing agent and preparation method thereof | |
| CN105801768B (en) | A kind of levelling agent in ramie fabric liquefied ammonia solvent dyeing and preparation method and application method | |
| CN101899228B (en) | Active yellow dye composition | |
| CN105908542B (en) | A kind of color fixing agent of ramie fabric liquefied ammonia solvent dyeing and preparation method and application method | |
| CN105350345A (en) | Ionic liquid dyeing method of reactive dyes | |
| CN101935466A (en) | Active red dye composition | |
| CN105778559A (en) | Black active dye composition and preparation method and use thereof | |
| CN101880473B (en) | Active orange dye composition | |
| CN104060485A (en) | Process of performing fixation on reactive dyed cotton fabric with reactive cationic color fixing agent | |
| CN102504102A (en) | 3-hydroxyazetidine reactive group-containing poly dimethyl diallyl ammonium chloride modified colouring stabilizer and synthesis method thereof | |
| CN105544245A (en) | Low-salt dyeing method for cotton fabrics | |
| CN105647238A (en) | Gray activated dye composition and preparation method as well as application thereof | |
| CN105778562A (en) | Black active dye composition and preparation method and use thereof | |
| CN102433030B (en) | Active yellow dye composition | |
| CN109267393B (en) | A kind of preparation method of the oil removing level dyeing compound emulsifying agent for dacron | |
| CN1322066C (en) | Composite active black dye | |
| CN102585548A (en) | Red active dye composition | |
| CN106752077B (en) | A kind of blue active dye composition and its preparation method and application | |
| CN105350329B (en) | A kind of polymer cation modifying agent for ramie fabric and preparation method and application method | |
| CN104231668A (en) | Preparation method and application of yellow reactive dye combination and fibers or fiber fabrics dyed with yellow reactive dye combination | |
| CN110205845A (en) | A kind of preparation method of New stablization | |
| CN108755198B (en) | Method for improving level-dyeing property of active blue on cotton fabric |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201201 Address after: No.716, 7th floor, building 4, No.99, Guangfu Road, Wuhou District, Chengdu City, Sichuan Province 610047 Patentee after: Chengdu yishenrui Technology Co.,Ltd. Address before: 430073 Wuhan Textile University, No. 1 Textile Road, Hongshan District, Hubei, Wuhan Patentee before: Wuhan Textile University Effective date of registration: 20201201 Address after: 313000 1-C, building 1, No. 656, Qixing Road, high tech Zone, Wuxing District, Huzhou City, Zhejiang Province Patentee after: Huzhou xinbeilian Network Technology Co.,Ltd. Address before: No.716, 7th floor, building 4, No.99, Guangfu Road, Wuhou District, Chengdu City, Sichuan Province 610047 Patentee before: Chengdu yishenrui Technology Co.,Ltd. |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230410 Address after: 621100 nansiba, Tongchuan Town, Santai County, Mianyang City, Sichuan Province Patentee after: Mianyang jialide Textile Technology Co.,Ltd. Address before: 313000 1-C, building 1, No. 656 Qixing Road, high tech Zone, Wuxing District, Huzhou City, Zhejiang Province Patentee before: Huzhou xinbeilian Network Technology Co.,Ltd. |