CN111519451A - Preparation method of printing paste - Google Patents

Preparation method of printing paste Download PDF

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Publication number
CN111519451A
CN111519451A CN202010184379.1A CN202010184379A CN111519451A CN 111519451 A CN111519451 A CN 111519451A CN 202010184379 A CN202010184379 A CN 202010184379A CN 111519451 A CN111519451 A CN 111519451A
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China
Prior art keywords
paste
printing
printing paste
reaction
prepared
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CN202010184379.1A
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Chinese (zh)
Inventor
何鑫
刘鹏远
厉安昕
张磊
单译
段福猛
庞磊
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Shenyang Institute Of Science And Technology
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Shenyang Institute Of Science And Technology
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Priority to CN202010184379.1A priority Critical patent/CN111519451A/en
Publication of CN111519451A publication Critical patent/CN111519451A/en
Pending legal-status Critical Current

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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/44General 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 insoluble pigments or auxiliary substances, e.g. binders
    • D06P1/46General 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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing natural macromolecular substances or derivatives thereof
    • D06P1/48Derivatives of carbohydrates
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/006Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
    • C08B37/0084Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/38General 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
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/58Material containing hydroxyl groups
    • D06P3/60Natural or regenerated cellulose
    • D06P3/66Natural or regenerated cellulose using reactive dyes

Abstract

A preparation method of printing paste belongs to the technical field of chemical printing and dyeing, and comprises the steps of using alginic acid and R-NH2、H2N‑R‑NH2And (R ═ alkyl, phenyl and carbonyl) or amine in polyamine is subjected to condensation reaction to generate amide alginate, the reaction temperature is 100-135 ℃, the reaction is carried out for 12-24h, after the reaction is finished, an ethanol solution is used for cleaning, and the product is dried at 85-100 ℃ to obtain the seaweed amide powder, namely the printing paste is prepared. The printing paste prepared by the method has the advantages of high solubility in water, good water-covering property, clear printing outline, high paste removal rate, soft hand feeling of the printed fabric after washing, good stability, obvious thickening effect and difficult hydrolysisAnd (3) dye printing paste.

Description

Preparation method of printing paste
Technical Field
The invention belongs to the technical field of chemical printing and dyeing, and particularly relates to a preparation method of printing paste.
Background
The printing paste is an important component of printing paste, and has great influence on printing pattern contour, vividness, uniformity, color supply amount and the like. The printing paste is a substance added in printing paste to play a thickening role, and generally can be dissolved in water or fully swelled and dispersed in water to form a colloidal solution. When the printing paste is prepared, the reactive dye is dissolved in water and then uniformly dispersed in the printing paste, namely the printing paste is a carrier of the paste. The printing paste for preparing the printing paste directly influences the printing quality, such as the technical indexes of color yield, printing definition, dye uptake and permeability, paste residue after printing and the like. Therefore, the printing paste plays an important role in printing production and is one of the main factors which restrict the product quality, the production cost and the economic benefit. At present, the printing paste mainly comprises seaweed, starch and cellulose modified substances, modified guar gum substances, synthetic thickeners and mineral thickeners. Since the advent of reactive dyes, sodium alginate has been the most commonly used paste in reactive dye printing. Because the natural polysaccharide carbohydrate alginic acid extracted from the kelp is insoluble in water and can not be used as an active printing paste, the alginic acid and sodium carbonate are subjected to neutralization reaction to generate strong-base weak-acid salt sodium alginate, although the sodium alginate has high solubility in water, good water-covering property, clear printing outline and high paste removal rate, the printed fabric after washing is soft in hand feeling, but is extremely easy to hydrolyze, the prepared color paste has short stabilization period during use, can be stored for only 2 days at normal temperature, and needs to be prepared and used in summer, thus being inconvenient and causing a great deal of waste. Sodium alginate is a strong base and weak acid salt substance, and can generate hydrolysis reaction after being dissolved in water to generate water-insoluble alginic acid, so that the thickening effect and the water retention of the alginic acid are deteriorated, and the reactive dye is separated out from printing paste to cause the failure of printing paste.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of printing paste, and the printing paste prepared by the method has the advantages of high solubility in water, good water-covering property, clear printing outline, high paste removal rate, soft hand feeling of the printed fabric after washing, good stability, obvious thickening effect and difficult hydrolysis.
The invention adopts the following technical scheme:
a process for preparing printing paste from alginic acid and R-NH2、H2N-R-NH2And (R ═ alkyl, phenyl and carbonyl) or amine in polyamine is subjected to condensation reaction to generate amide alginate, the reaction temperature is 100-135 ℃, the reaction is carried out for 12-24h, after the reaction is finished, an ethanol solution is used for cleaning, and the product is dried at 85-100 ℃ to obtain the seaweed amide powder, namely the printing paste is prepared.
Further, the method specifically comprises the step of reacting alginic acid with ethylenediamine, ethylamine and p-phenylenediamine, wherein the alginic acid, the ethylamine and H2N-R-NH2The mass ratio of the p-phenylenediamine is 1: 1-1: 5.
The invention has the advantages and effects that:
the invention uses alginic acid and R-NH2、H2N-R-NH2The (R ═ alkyl, phenyl and carbonyl) or the amine group in the polyamine are subjected to condensation reaction to generate the amide alginate, and the printing paste of the alginate reactive dye has good stability, high viscosity, high paste removal rate and good printing uniformity.
Drawings
FIG. 1 is a schematic representation of the overall reaction equation;
FIG. 2 is a graph of the viscosities and changes thereof of example 1, example 2, example 3 and comparative example 1;
FIG. 3 is a K/S data distribution diagram of application example 1;
FIG. 4 is a K/S data distribution diagram of application example 2;
FIG. 5 is a K/S data distribution diagram of application example 3;
FIG. 6 is a K/S data distribution diagram of comparative example 2;
FIG. 7 is an attenuated Total reflectance IR spectrum of the product of example 1.
Detailed Description
The invention is further explained below with reference to the figures and the examples.
Alginic acid is an organic acid, the carboxyl group of which can react with R-NH under the action of heat or acid catalyst2、H2N-R-NH2(R ═ alkyl, phenyl, etc.) and other amine groups in polyamine are condensated to produce amide alginate, which is prepared with 0.2-2 wt% sulfuric acid or phosphoric acid as catalyst and at 100-135 deg.c2N-R-NH2P-phenylenediamine and the like are reacted for 12 to 24 hours according to the mass ratio of 1: 1 to 1: 5, ethanol solution is used for cleaning after the reaction is finished, and the product is dried at the temperature of 85 to 100 ℃ to obtain the seaweed amide powder.
Example 1
1) Adding 9.04g of ethylenediamine into 100g of 15 wt% alginic acid slurry under stirring, uniformly mixing, and stirring and refluxing for 12-24h at the reaction temperature of 120-135 ℃.
2) Washing the product obtained after the reaction in the step 1) with absolute ethyl alcohol for 3-4 times, recovering the washing liquid, drying the washed product at the temperature of 85-100 ℃, and removing the excessive ethyl alcohol to obtain the ethylenediamine alginate powder.
Preparing the powder obtained in the step 2) into a paste with the mass fraction of 2%, and measuring the viscosity by using a viscometer, wherein the higher the viscosity is, the better the paste forming property is. The paste is kept at the constant temperature of 60 ℃ for 24 hours, and the viscosity is measured every 4 hours. The change in viscosity of the paste was followed, with smaller viscosity changes indicating better paste stability.
Example 2
1) Adding 8.5g of ethylamine into 15 wt% of alginic acid slurry while stirring, uniformly mixing, and stirring and refluxing for 12-24h at the reaction temperature of 120-135 ℃.
2) Washing the product obtained after the reaction in the step 1) with absolute ethyl alcohol for 3-4 times, recovering the washing liquid, drying the washed product at the temperature of 85-100 ℃, and removing the excessive ethyl alcohol to obtain the ethylamine alginate powder.
Preparing the powder obtained in the step 2) into a paste with the mass fraction of 2%, and measuring the viscosity by using a viscometer, wherein the higher the viscosity is, the better the paste forming property is. The paste is kept at the constant temperature of 60 ℃ for 24 hours, and the viscosity is measured every 4 hours. The change in viscosity of the paste was followed, with smaller viscosity changes indicating better paste stability.
Example 3
1) Adding 15g of p-phenylenediamine into 11 wt% of alginic acid slurry while stirring, uniformly mixing, and stirring and refluxing for 18-24 h at the reaction temperature of 100-135 ℃.
2) Washing the product obtained after the reaction in the step 1) with absolute ethyl alcohol for 3-4 times, recovering the washing liquid, drying the washed product at the temperature of 85-100 ℃, and removing the redundant ethyl alcohol to obtain the alginic acid p-phenylenediamine salt solid.
Preparing the powder obtained in the step 3) into a paste with the mass fraction of 2%, and measuring the viscosity by using a viscometer, wherein the higher the viscosity is, the better the paste forming property is. The paste is kept at the constant temperature of 60 ℃ for 24 hours, and the viscosity is measured every 4 hours. The change in viscosity of the paste was followed, with smaller viscosity changes indicating better paste stability.
Comparative example 1
Preparing the sodium alginate powder into a paste with the mass fraction of 2%, and measuring the viscosity by using a viscometer, wherein the higher the viscosity is, the better the paste forming property is. The paste is kept at the constant temperature of 60 ℃ for 24 hours, and the viscosity is measured every 4 hours. The change in viscosity of the paste was followed, with smaller viscosity changes indicating better paste stability.
As can be seen from FIG. 2, the pasty property and viscosity stability of the seaweed amine paste synthesized by the invention are superior to those of sodium alginate.
Application example 1
1 wt% of urea, 2.5 wt% of baking soda, 0.5 wt% of anti-staining salt s and 5 wt% of reactive K dye turquoise blue SPE were accurately weighed, dissolved in 30 wt% of deionized water, added with 50 wt% of the paste prepared in example 1, stirred and stirred uniformly.
The prepared color paste is printed on pure cotton fabric, and the specific process is as follows: pure cotton fabric → printing paste (5mm/s, 3V) → drying (80-85 ℃, 3-4min) → steaming (101-.
And (5) measuring the color uniformity of the printed cloth surface. The cloth sample printed by the process is tested and analyzed by a Datacolor SF600X color measuring instrument of Datacolor company in America, and the data of 16-point color yield (K/S value) of the printed cloth surface which is random and uniform is obtained. The more concentrated the distribution of K/S values is, the better the color uniformity of the printed cloth surface is; on the contrary, the wider the distribution of K/S value, the worse the color uniformity of the printed cloth surface. The K/S data distribution is shown in FIG. 3.
Application example 2
2 wt% of urea, 2.5 wt% of baking soda, 0.5 wt% of anti-staining salt s and 5 wt% of reactive K dye turquoise blue SPE were accurately weighed, dissolved in 30 wt% of deionized water, added with 50 wt% of the paste prepared in example 2, stirred and stirred uniformly.
The prepared color paste is printed on pure cotton fabric, and the specific process is as follows: pure cotton fabric → printing paste (5mm/s, 3V) → drying (80-85 ℃, 3-4min) → steaming (101-.
And (5) measuring the color uniformity of the printed cloth surface. The cloth sample printed by the process is tested and analyzed by a Datacolor SF600X color measuring instrument of Datacolor company in America, and the data of 16-point color yield (K/S value) of the printed cloth surface which is random and uniform is obtained. The more concentrated the distribution of K/S values is, the better the color uniformity of the printed cloth surface is; on the contrary, the wider the distribution of K/S value, the worse the color uniformity of the printed cloth surface. The K/S data distribution is shown in FIG. 4.
Application example 3
2.5 wt% of urea, 2.5 wt% of baking soda, 0.5 wt% of dye-repellent salt s and 5 wt% of reactive K dye turquoise blue SPE were accurately weighed, dissolved in 30 wt% of deionized water, added with 50 wt% of the paste prepared in example 3, stirred and stirred uniformly.
The prepared color paste is printed on pure cotton fabric, and the specific process is as follows: pure cotton fabric → printing paste (5mm/s, 3V) → drying (80-85 ℃, 3-4min) → steaming (101-.
And (5) measuring the color uniformity of the printed cloth surface. The cloth sample printed by the process is tested and analyzed by a Datacolor SF600X color measuring instrument of Datacolor company in America, and the data of 16-point color yield (K/S value) of the printed cloth surface which is random and uniform is obtained. The more concentrated the distribution of K/S values is, the better the color uniformity of the printed cloth surface is; on the contrary, the wider the distribution of K/S value, the worse the color uniformity of the printed cloth surface. The K/S data distribution is shown in FIG. 5.
Comparative example 2
10 wt% of urea, 2.5 wt% of baking soda, 0.5 wt% of anti-staining salt s and 5 wt% of reactive K-type dye turquoise blue SPE were accurately weighed, dissolved in 30 wt% of deionized water, added with 50 wt% of the paste prepared in comparative example 1, stirred and stirred uniformly.
The prepared color paste is printed on pure cotton fabric, and the specific process is as follows: pure cotton fabric → printing paste (5mm/s, 3V) → drying (80-85 ℃, 3-4min) → steaming (101-.
And (5) measuring the color uniformity of the printed cloth surface. The cloth sample printed by the process is tested and analyzed by a Datacolor SF600X color measuring instrument of Datacolor company in America, and the data of 16-point color yield (K/S value) of the printed cloth surface which is random and uniform is obtained. The more concentrated the distribution of K/S values is, the better the color uniformity of the printed cloth surface is; on the contrary, the wider the distribution of K/S value, the worse the color uniformity of the printed cloth surface. The K/S data distribution is shown in FIG. 6.
As is clear from FIGS. 3, 4, 5 and 6, the seaweed amide based paste synthesized by the present invention has better color uniformity than the sodium alginate paste.

Claims (2)

1. A preparation method of printing paste is characterized by comprising the following steps: the method is to use alginic acid and R-NH2、H2N-R-NH2And (R ═ alkyl, phenyl and carbonyl) or amine in polyamine is subjected to condensation reaction to generate amide alginate, the reaction temperature is 100-135 ℃, the reaction is carried out for 12-24h, after the reaction is finished, an ethanol solution is used for cleaning, and the product is dried at 85-100 ℃ to obtain the seaweed amide powder, namely the printing paste is prepared.
2. The method for preparing a printing paste according to claim 1, wherein: the method specifically comprises the step of reacting alginic acid with ethylenediamine, ethylamine and p-phenylenediamine, wherein the alginic acid, the ethylamine, H2N-R-NH2 and the p-phenylenediamine are in a mass ratio of 1: 1-1: 5.
CN202010184379.1A 2020-03-06 2020-03-06 Preparation method of printing paste Pending CN111519451A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113861308A (en) * 2021-10-20 2021-12-31 北京服装学院 Modified alginic acid derivative and application thereof as pretreatment agent for digital printing of cotton fabrics
CN114437246A (en) * 2022-02-18 2022-05-06 山东海基生物科技有限公司 Method for improving viscosity of sodium alginate

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008127718A (en) * 2006-11-22 2008-06-05 Tokai Senko Kk Method for producing printed textile product
CN103556502A (en) * 2013-11-19 2014-02-05 青岛明月海藻集团有限公司 Additive of printing paste as well as preparation method and using method of additive
CN110106728A (en) * 2019-05-08 2019-08-09 安徽省翰先纺织科技有限公司 Pigment printing technique

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008127718A (en) * 2006-11-22 2008-06-05 Tokai Senko Kk Method for producing printed textile product
CN103556502A (en) * 2013-11-19 2014-02-05 青岛明月海藻集团有限公司 Additive of printing paste as well as preparation method and using method of additive
CN110106728A (en) * 2019-05-08 2019-08-09 安徽省翰先纺织科技有限公司 Pigment printing technique

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113861308A (en) * 2021-10-20 2021-12-31 北京服装学院 Modified alginic acid derivative and application thereof as pretreatment agent for digital printing of cotton fabrics
CN114437246A (en) * 2022-02-18 2022-05-06 山东海基生物科技有限公司 Method for improving viscosity of sodium alginate
CN114437246B (en) * 2022-02-18 2023-02-03 山东海基生物科技有限公司 Method for improving viscosity of sodium alginate

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Application publication date: 20200811

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