CN103450413B - A kind of thickening material for printing in textiles and preparation method thereof - Google Patents
A kind of thickening material for printing in textiles and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of thickening material for printing in textiles and preparation method thereof, belong to textile finishing processing technique field.By the vinylformic acid of certain mass and N, N '-methylene-bisacrylamide adds in reactor, and being neutralized to pH with ammoniacal liquor or sodium hydroxide solution is 6.3 ~ 6.8; Add the mixed solution of Arlacel-80 and kerosene again, stir, slowly add modified chitosan and catalyzer, after fully emulsified one-tenth thick liquid, pass into nitrogen, heating, after reaction terminates, cool the temperature to room temperature; Finally add tween-80, after abundant rp-emulsification, namely obtain a kind of electrolyte-resistant thickener, for the pigment printing of textiles, Disperse Printing and printing with reactive dye.The present invention adopts maleic anhydride modified chitosan as the function monomer improving thickening material electrolyte res is tance, and raw material sources are extensive, and preparation technology is simple, be easy to control, and is applicable to suitability for industrialized production.
Description
Technical field
The present invention relates to a kind of synthesis of printing in textiles thickening material, be specifically related to a kind of electrolyte-resistant thickener comprising modified chitosan and preparation method thereof.
Background technology
Thickening material is indispensable auxiliary agent in printing in textiles mill base, thickening material gives printing paste certain viscosity, reduces its rheological, ensures carrying out smoothly of stamp processing, can also the imbibition that causes of partial offset fabric capillary effect, thus ensure the clear-cut of decorative pattern.Before synthetic thickening agent does not occur, textile printing uses the natural thickener of natural thickener or modification, as sodium alginate, starch, Mierocrystalline cellulose, natural gum and so on etc., but natural thickening material has some intrinsic shortcomings, as poor in hydration time length, thermostability and shear flow sex change etc.Therefore, in current stamp industry, the general synthetic thickening agent that adopts substitutes, synthetic thickening agent is developed so far with the thickening capabilities of anionic polyacrylate the strongest, but the electrolyte-resistant effect of Polyacrylic Acid Thickener is poor, and in most of the cases there is a large amount of ionogen in printing in textiles mill base, common thickening material can not meet the demands.Therefore, in order to meet the demand of market to high quality, high benefit stamp, the Polyacrylic Acid Thickener that exploitation electrolyte-resistant ability is strong has very important significance.
At present, the research of domestic and international thickening material is all what to improve the thickening capabilities of thickening material and electrolyte-resistant ability be main research.US Patent No. 4814096 discloses a kind of acrylamide, vinylformic acid, lauryl methacrylate multipolymer, there is the characteristic of heatproof electrolyte-resistant, but the ester of hydrophobicity long-chain (lauryl methacrylate) facile hydrolysis in the basic conditions, association effect can be affected, electrolyte res is tance is affected; Chinese invention patent CN1624237A discloses a kind of Acrylic Acid Monomer class thickening material utilizing reversed emulsion polymerization to prepare, although electrolyte res is tance increases, thickening effectiveness is limited; Publication number is that the Chinese invention patent of CN101886345A, CN101736608A and CN101775099A utilizes reversed-phase emulsion copolymerization method to prepare anionic acrylic monomer class thickening material, polyether segment is introduced at its molecule segment, its electrolyte-resistant ability is increased, but their synthesis technique is more complicated, and condition is wayward.
Summary of the invention
The object of this invention is to provide a kind of electrolyte res is tance to stablize and effective Polyacrylic Acid Thickener and preparation method thereof, the requirement of textile coating stamp, Disperse Printing and printing with reactive dye can be met, there is again the feature of high performance-price ratio.
In order to achieve the above object, the technical solution used in the present invention is to provide a kind of preparation method of the thickening material for printing in textiles, comprises the steps:
1, by N, N, '-methylene-bisacrylamide join in vinylformic acid, N, N '-methylene-bisacrylamide quality is 1 ~ 1.5% of vinylformic acid quality, drips sodium hydroxide or ammonia soln, obtain the mixed solution that pH is 6.3 ~ 6.8 under agitation condition;
2, the kerosene accounting for vinylformic acid quality 60 ~ 70% is taken, add the Arlacel-80 accounting for kerosene quality 10 ~ 15%, after stirring, the mixed solution obtained with step 1 again, account for the modified chitosan of vinylformic acid quality 1.2% ~ 1.5% and account for the Potassium Persulphate of vinylformic acid quality 0.2 ~ 0.4%, low whipping speed is the emulsified process of condition 40 ~ 60 minutes of 1000 ~ 1300 revs/min, obtains the liquid of thickness;
3, thick liquid low whipping speed step 2 obtained is 250 ~ 300 revs/min, nitrogen atmosphere, temperature are react after 2 ~ 3 hours under the condition of 60 ~ 65 DEG C, cool the temperature to room temperature, add the tween-80 with Arlacel-80 equal in quality, low whipping speed is that under the condition of 700 ~ 1000 revs/min, rp-emulsification process, after 30 ~ 40 minutes, obtains a kind of thickening material for printing in textiles.
Described modified chitosan preparation method is: chitosan being joined massfraction is in the acetic acid solution of 2%, is stirred to formation homogeneous phase solution; Be dissolved in acetone by maleic anhydride, then join in this homogeneous phase solution, maleic anhydride quality is 3 ~ 5% of chitosan mass; Under the condition that room temperature also constantly stirs, reaction is after 10 ~ 12 hours, and purified product, obtains modified chitosan.
Technical solution of the present invention also comprises a kind of thickening material for printing in textiles obtained by above-mentioned preparation method, and uses it in the mill base of the pigment printing of textiles, Disperse Printing and printing with reactive dye.
Principle of the present invention is: adopt maleic anhydride modified chitosan, introduce carbon-carbon double bond on the one hand, make modification chitosan can with vinylformic acid generation copolyreaction, utilize chitosan molecule simultaneously containing multiple hydrophilic radicals such as hydroxyl, kharophen and amino, and the mutual synergistic effect between these hydrophilic radicals significantly can improve the water absorbent rate of thickening material; On the other hand, the introducing of carboxyl groups, makes the hydrophobic interaction of an interchain be strengthened, due to the heat resistance and salt tolerance between polymer molecule, macromolecular chain can be made to be cross-linked to form the space net structure had to a certain degree, to improve the electrolyte-resistant ability of thickening material; Therefore, adopt technical solution of the present invention, not only can improve thickening capabilities but also electrolyte-resistant ability can be improved.
Due to the utilization of technique scheme, the present invention compared with prior art tool has the following advantages:
1, the maleic anhydride modified chitosan of the present invention's employing is as the function monomer improving thickening material electrolyte-resistant ability, introduces double bond on the one hand, makes chitosan and acrylic acid copolymer, improves thickening capabilities; Introduce carboxyl groups on the other hand, the hydrophobic interaction of an interchain is strengthened, due to the heat resistance and salt tolerance between polymer molecule, macromolecular chain can be made to be cross-linked to form the space net structure had to a certain degree, the electrolyte-resistant ability of thickening material can be improved.
2, present invention employs the chitosan of modification as the function monomer improving electrolyte-resistant ability, and chitosan itself belongs to the natural high moleculer eompound of biocompatibility, and readily biodegradable.
3, the electrolyte-resistant thickener that the present invention obtains can meet the requirement of textile coating stamp, Disperse Printing and printing with reactive dye, has again the feature of high performance-price ratio.
4, present invention process is simple, is easy to control, and is applicable to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the comparative graph of the acid and alkali-resistance ability of the thickening material that provides of the embodiment of the present invention 1,2 and 3 and common commercially available thickening material;
Fig. 2 is the comparative graph of the salt resistance ability of the thickening material that provides of the embodiment of the present invention 1,2 and 3 and common commercially available thickening material;
Fig. 3 ~ Fig. 5 is the infrared spectrogram of chitosan, modified chitosan and the electrolyte-resistant thickener that the embodiment of the present invention 1,2 and 3 provides respectively.
Embodiment
Below in conjunction with drawings and Examples, technical solution of the present invention will be further described.
Embodiment 1
Take 10g chitosan and be placed in reactor, add the acetic acid solution that massfraction is 2%, be stirred to formation homogeneous phase solution; Take 0.3g maleic anhydride, be dissolved in acetone, then join in this reactor, under the condition that room temperature also constantly stirs, reaction is after 10 hours, and purified product, obtains modified chitosan.
Join in reactor by 60g vinylformic acid and 0.6g N, N '-methylene-bisacrylamide, being neutralized to pH with sodium hydroxide solution is 6.3; Take 40g kerosene and 5g Arlacel-80 again, to add after both are fully mixed in vinylformic acid and after mixed solution in; Add 0.72g modified chitosan and 0.12g Potassium Persulphate again, when rotating speed is 1200 revs/min fully emulsified 50 minutes.
Changing rotating speed is 250 revs/min, passes into nitrogen, and temperature is controlled after 3 hours 60 DEG C of reactions, to be down to room temperature, to add 5g tween-80, stirs 35 minutes, obtain a kind of electrolyte-resistant thickener under the speed of 800 revs/min.
Embodiment 2
Take 10g chitosan and be placed in reactor, add the acetic acid solution that massfraction is 2%, be stirred to formation homogeneous phase solution; Take 0.4g maleic anhydride, be dissolved in acetone, then join in this reactor, under the condition that room temperature also constantly stirs, reaction is after 11 hours, and purified product, obtains modified chitosan.
Join in reactor by 60g vinylformic acid and 0.78g N, N '-methylene-bisacrylamide, being neutralized to pH with sodium hydroxide solution is 6.5; Take 36g kerosene and 3.6g Arlacel-80 again, to add after both are fully mixed in vinylformic acid and after mixed solution in; Add 0.8g modified chitosan and 0.18g Potassium Persulphate again, when rotating speed is 1100 revs/min fully emulsified 60 minutes.
Changing rotating speed is 280 revs/min, passes into nitrogen, and temperature is controlled after 2 hours 65 DEG C of reactions, to be down to room temperature, to add 3.6g tween-80, stirs 40 minutes, obtain a kind of electrolyte-resistant thickener under the speed of 700 revs/min.
Embodiment 3
Get 10g chitosan and be placed in reactor, add the acetic acid solution that massfraction is 2%, be stirred to formation homogeneous phase solution; Take 0.5g maleic anhydride, be dissolved in acetone, then join in this reactor, under the condition that room temperature also constantly stirs, reaction is after 12 hours, and purified product, obtains modified chitosan.
Joining in reactor by 60g vinylformic acid and 0.9g N, N '-methylene-bisacrylamide, is 6.8 with ammonia neutralization to pH; Take 42g kerosene and 6.3g Arlacel-80 again, to add after both are fully mixed in vinylformic acid and after mixed solution in; Add 0.9g modified chitosan and 0.24g Potassium Persulphate again, when rotating speed is 1300 revs/min fully emulsified 40 minutes.
Changing rotating speed is 300 revs/min, passes into nitrogen, and temperature is controlled after 2.5 hours 63 DEG C of reactions, to be down to room temperature, to add 6.3g tween-80, stirs 30 minutes, obtain a kind of electrolyte-resistant thickener under the speed of 900 revs/min.
The electrolyte-resistant thickener of the embodiment of the present invention 1 ~ 3 is carried out electrolyte res is tance test, and the thickening material M conventional with current print works carries out effect comparison, concrete testing method and result as follows:
1, the mensuration of acid-proof alkaline
The thickening material prepare embodiment 1, embodiment 2, embodiment 3 and commercially available thickening material M are made into the white slurry of 3% respectively, and the pH value of white slurry is regulated with sodium hydroxide or acetic acid, then measure the viscosity starched in vain when pH value is 3,5,7,9 and 11, result as shown in Figure 1.
2, the mensuration of salt resistant character
The thickening material prepare embodiment 1,2 and 3 and commercially available thickening material M are made into the white slurry of 3% respectively, then by the massfraction of preparation be 0.1% NaCl solution be added drop-wise to above-mentioned thickening material starch in vain in (adding 1g) at every turn, stir, measure the viscosity of starching in vain when NaCl solution is 1g, 2g, 3g, 4g, 5g, 6g, 7g, 8g, 9g and 10g, result as shown in Figure 2.
See accompanying drawing 1, it is that the acid and alkali-resistance ability of four kinds of thickening materials that the present embodiment provides compares; As shown in Figure 1, with regard to acid-fast ability, the acid-fast ability of thickening material M is suitable with embodiment 3, is better than embodiment 1; The resistance to alkali ability of thickening material M is better than embodiment 1 and embodiment 3.But the acid-fast ability of embodiment 2 and resistance to alkali ability are all better than thickening material M.
See accompanying drawing 2, the salt resistance ability of four kinds of thickening materials compares; As shown in Figure 2, the salt resistance ability of embodiment 2 is better than thickening material M.
The electrolyte-resistant thickener that the embodiment of the present invention 1 ~ 3 provides is respectively used to the test of pigment printing, Disperse Printing and printing with reactive dye, its quality measurements is as follows:
1, pigment printing
Material: polyester-cotton blend bleached woven fabric, coating is red, water polyacrylic acid tackiness agent, thickening material.
Coating prescription:
The red 3g of coating
Tackiness agent 15g
Thickening material 3g
Mill base total amount 100g after adding water
Printing technology flow process:
Tinting paste → stamp → oven dry (80 DEG C, 3min) → bake (150 DEG C, 3min)
Printing quality measuring method
(1) K/S value, rate of permeation and uneven shade degree: the K/S value measuring PRINTED FABRIC decorative pattern place with electronics color measurement and color match instrument, rate of permeation is calculated as follows:
Select nine place's PRINTED FABRIC to measure corresponding K/S value, calculating mean value, and be calculated as follows uneven shade degree, less then the printed fabric color of this value is more even.
(2) de-paste rate: PRINTED FABRIC is containing soap flakes 2g/L, Na
2cO
3with 95 DEG C of 20min that soap, bath raio 1:50 in the solution of 2g/L, then through hot water wash, cold wash, dry.De-paste rate is calculated as follows:
(3) PRINTED FABRIC colour fastness: dry, the fastness to wet rubbing measuring DYED FABRICS by GB/T 3920-1997 " textile color stability test colour fastness to rubbing ".
Produce upper conventional certain factory thickening material M for comparative example with current enterprise stamp, the thickening material provided with the embodiment of the present invention 1 ~ 3 compares, as shown in table 1 by the quality determination result after above-mentioned processing condition stamp.
The performance of fabric after table 1 stamp
| Sample | Dry fastness/level | Fastness to wet rubbing/level | K/S value | De-paste rate/% | Rate of permeation/% | Uneven shade degree |
| Embodiment 1 | 4～5 | 3～4 | 11.33 | 78.75 | 61.62 | 0.066 |
| Embodiment 2 | 4～5 | 3～4 | 12.13 | 80.16 | 64.63 | 0.047 |
| Embodiment 3 | 4～5 | 3～4 | 11.39 | 77.09 | 53.53 | 0.050 |
| Thickening material M | 4～5 | 3～4 | 10.98 | 77.88 | 62.74 | 0.055 |
As shown in Table 1, the dye yield of embodiment 1 ~ 3 sample is all better than thickening material M, and the de-paste rate of embodiment 2, rate of permeation and uneven shade degree are all better than thickening material M.
2, Disperse Printing
Material: polyester piece good, Disperse Red, thickening material, linking agent
Prescription stuck with paste by stamp:
Disperse Red 2g
Linking agent 6g
Thickening material 5g
After adding water, total amount 100g stuck with paste by stamp
Printing technology flow process:
Modulation mill base → stamp → oven dry (80 DEG C, 3min) → decatize (170 DEG C, 6min) → washing → reduction clearing) → washing → dry
Printing quality measuring method
(1) K/S value, rate of permeation and uneven shade degree: the K/S value measuring PRINTED FABRIC decorative pattern place with electronics color measurement and color match instrument, rate of permeation is calculated as follows:
Select nine place's PRINTED FABRIC to measure corresponding K/S value, calculating mean value, and be calculated as follows uneven shade degree, less then the printed fabric color of this value is more even.
(2) de-paste rate: PRINTED FABRIC is containing soap flakes 2g/L, Na
2cO
3with 95 DEG C of 20min that soap, bath raio 1:50 in the solution of 2g/L, then through hot water wash, cold wash, dry.De-paste rate is calculated as follows:
(3) PRINTED FABRIC colour fastness: dry, the fastness to wet rubbing measuring DYED FABRICS by GB/T 3920-1997 " textile color stability test colour fastness to rubbing ".
Produce upper conventional certain factory thickening material M for comparative example with current enterprise stamp, the thickening material provided with the embodiment of the present invention 1 ~ 3 compares, as shown in table 2 by the quality determination result after above-mentioned processing condition stamp.
The performance of fabric after table 2 stamp
| Sample | Dry fastness/level | Fastness to wet rubbing/level | K/S value | De-paste rate/% | Rate of permeation/% | Uneven shade degree |
| Embodiment 1 | 4～5 | 3～4 | 12.628 | 67.23 | 22.89 | 0.104 |
| Embodiment 2 | 4～5 | 3～4 | 13.071 | 70.33 | 29.71 | 0.078 |
| Embodiment 3 | 4～5 | 3～4 | 12.723 | 68.69 | 21.57 | 0.083 |
| Thickening material M | 4～5 | 3～4 | 12.118 | 70.06 | 27.23 | 0.085 |
As shown in Table 2, the dye yield of embodiment 1 ~ 3 sample is all higher than thickening material M, and the de-paste rate of embodiment 2, rate of permeation and uneven shade degree are all better than thickening material M.
3, printing with reactive dye
Material: pure cotton fabric, reactive red, thickening material, urea, soda ash, reservehao S.
Prescription stuck with paste by stamp:
Reactive red 3g
Urea 4g
Soda ash 2g
Reservehao S 1g
Thickening material 5g
After adding water, total amount 100g stuck with paste by stamp
Printing technology flow process:
Modulation mill base → stamp → oven dry (60 DEG C) → decatize (102 ~ 103 DEG C, 10min) → cold wash → hot water wash → soap boiling (soap flakes 2g/L, bath raio 1:50,95 DEG C, 10min) → hot water wash → cold wash → oven dry
Printing quality measuring method
(1) K/S value, rate of permeation and uneven shade degree: the K/S value measuring PRINTED FABRIC decorative pattern place with electronics color measurement and color match instrument, rate of permeation is calculated as follows:
Select nine place's PRINTED FABRIC to measure corresponding K/S value, calculating mean value, and be calculated as follows uneven shade degree, less then the printed fabric color of this value is more even.
(2) de-paste rate: PRINTED FABRIC is containing soap flakes 2g/L, Na
2cO
3with 95 DEG C of 20min that soap, bath raio 1:50 in the solution of 2g/L, then through hot water wash, cold wash, dry.De-paste rate is calculated as follows:
(3) PRINTED FABRIC colour fastness: dry, the fastness to wet rubbing measuring DYED FABRICS by GB/T 3920-1997 " textile color stability test colour fastness to rubbing ".
The performance of fabric after table 3 stamp
| Sample | Dry fastness/level | Fastness to wet rubbing/level | K/S value | De-paste rate/% | Rate of permeation/% | Uneven shade degree |
| Embodiment 1 | 4～5 | 3～4 | 18.339 | 76.74 | 71.17 | 0.097 |
| Embodiment 2 | 4～5 | 4 | 19.078 | 78.76 | 73.78 | 0.064 |
| Embodiment 3 | 4～5 | 3～4 | 15.125 | 73.61 | 70.10 | 0.077 |
| Thickening material M | 4～5 | 3～4 | 12.252 | 70.03 | 69.25 | 0.068 |
As shown in Table 3, the dye yield of embodiment 1 ~ 3 sample, de-paste rate and rate of permeation are all better than thickening material M, and the uneven shade degree of embodiment 2 is also better than thickening material M.
Infrared spectroscopy
In the embodiment of the present invention 1 ~ 3, the infrared spectrum of chitosan, modified chitosan and electrolyte-resistant thickener is respectively see shown in accompanying drawing 3,4 and 5.Accompanying drawing 3 is the infrared spectrogram of the electrolyte-resistant thickener of embodiment 1; Accompanying drawing 4 is the infrared spectrogram of the electrolyte-resistant thickener of embodiment 2; Accompanying drawing 5 is the infrared spectrogram of the electrolyte-resistant thickener of embodiment 3; In each figure, curve 1 is chitosan, and curve 2 is modified chitosan, and curve 3 is electrolyte-resistant thickener.
As can be seen from Fig. 3, Fig. 4 and Fig. 5, in embodiment 1 ~ 3, each absorption peak position of modified chitosan (curve 2) is roughly the same.Curve 2 is at 3446.17 cm
-1the stretching vibration peak of place O-H is obviously strengthened; At 1629.77 cm
-1there is new peak in place, is the stretching vibration peak of C=C; At 1702.16 cm
-1also there is new peak in place, is the stretching vibration peak of C=O in-COOH.Illustrate that maleic anhydride take part in reaction, successful modification chitosan.2926.26 cm in curve 3
-1place is C-H stretching vibration on alkyl; 1408.20 cm
-1and 1559.571cm
-1the new peak that place occurs is-COO in carboxylic acid ionogen
-characteristic peak; 1658.28 cm
-1place is the stretching vibration peak of C=C.Illustrate that modified chitosan take part in crosslinking reaction.
Claims (3)
1., for a preparation method for the thickening material of printing in textiles, it is characterized in that comprising the steps:
(1) by N, N, '-methylene-bisacrylamide join in vinylformic acid, N, N '-methylene-bisacrylamide quality is 1 ~ 1.5% of vinylformic acid quality, drips sodium hydroxide or ammonia soln, obtain the mixed solution that pH is 6.3 ~ 6.8 under agitation condition;
(2) kerosene accounting for vinylformic acid quality 60 ~ 70% is taken, add the Arlacel-80 accounting for kerosene quality 10 ~ 15%, after stirring, the mixed solution obtained with step (1) again, the modified chitosan accounting for vinylformic acid quality 1.2% ~ 1.5% and account for the Potassium Persulphate of vinylformic acid quality 0.2 ~ 0.4%, low whipping speed is the emulsified process of condition 40 ~ 60 minutes of 1000 ~ 1300 revs/min, obtains the liquid of thickness; Described modified chitosan preparation method is: chitosan being joined massfraction is in the acetic acid solution of 2%, is stirred to formation homogeneous phase solution; Be dissolved in acetone by maleic anhydride, then join in this homogeneous phase solution, maleic anhydride quality is 3 ~ 5% of chitosan mass; Under the condition that room temperature also constantly stirs, reaction is after 10 ~ 12 hours, and purified product, obtains modified chitosan;
(3) be 250 ~ 300 revs/min by the thick liquid low whipping speed that step (2) obtains, nitrogen atmosphere, temperature be react after 2 ~ 3 hours under the condition of 60 ~ 65 DEG C, cool the temperature to room temperature, add the tween-80 with Arlacel-80 equal in quality, low whipping speed is that under the condition of 700 ~ 1000 revs/min, rp-emulsification process, after 30 ~ 40 minutes, obtains a kind of thickening material for printing in textiles.
2. by a kind of thickening material for printing in textiles that claim 1 preparation method obtains.
3. by a kind of thickening material for printing in textiles that claim 1 preparation method obtains, in the mill base for the pigment printing of textiles, Disperse Printing and printing with reactive dye.
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| CN104356300B (en) * | 2014-10-22 | 2017-03-29 | 陕西科技大学 | Efficient retardation water reducing agent of a kind of modification of chitosan and preparation method thereof and using method |
| CN105714579B (en) * | 2016-02-25 | 2018-03-16 | 东莞市联洲知识产权运营管理有限公司 | A kind of reactive dye environmental soft printing thickening agent and preparation method thereof |
| CN109355945A (en) * | 2018-09-21 | 2019-02-19 | 佛山市森昂生物科技有限公司 | A kind of printing thickening agent |
| CN113336903A (en) * | 2021-05-18 | 2021-09-03 | 林光亮 | Composite thickening agent for paint and preparation method thereof |
| CN114276492B (en) * | 2022-01-19 | 2023-11-28 | 广东星狮能源科技有限公司 | Ultraviolet-resistant thickener, preparation method thereof and disinfection no-wash hand-rubbing gel |
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| TR01 | Transfer of patent right |
Effective date of registration: 20190524 Address after: 215200 Hehua Village Group 2, Shengze Town, Wujiang District, Suzhou City, Jiangsu Province Patentee after: Suzhou Jinglai Textile Finishing Co., Ltd. Address before: 215228 No. 1188 west two ring road, Shengze Town, Wujiang District, Suzhou, Jiangsu. Patentee before: Suzhou Shengze science and Technology Pioneer Park Development Co., Ltd. |
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| TR01 | Transfer of patent right |