阅读说明：本技术 一种印花糊料的制备方法 (Preparation method of printing paste ) 是由 陈根旺 于 2020-06-03 设计创作，主要内容包括：本发明涉及一种印花糊料的制备方法,属于纺织印染类技术领域。本发明首先将木质素利用碱性溶液进行碱化处理,并且加入表面活性剂增强活性,再与环糊精与海藻酸钠进行混合,在复合溶液的环境下,通过还原剂及引发剂的作用,与添加剂进行反应,通过引发剂的作用进行聚合,形成碱性木质素接枝聚合物,而且对海藻酸钠进行了部分包裹,提高了成糊效率,同时渗透性能及结合性能,再通过氨基磺酸对其中物质进行磺化处理,增加了溶解性能,提高流动性能,使用甲醛进行甲基化处理,最后与淀粉、环氧氯丙烷进行混合,再碱性溶液中进行交联反应,增强了化学稳定性,脱糊性能,增强了成糊效率。本发明解决了目前印花糊料渗透性不好,成糊率低的问题。(The invention relates to a preparation method of printing paste, belonging to the technical field of textile printing and dyeing. According to the invention, firstly, lignin is subjected to alkalization treatment by using an alkaline solution, a surfactant is added to enhance activity, and then the lignin is mixed with cyclodextrin and sodium alginate, the lignin is reacted with an additive under the action of a reducing agent and an initiator in a composite solution environment, the reaction is carried out through the initiator, the polymerization is carried out through the action of the initiator to form an alkaline lignin graft polymer, the sodium alginate is partially wrapped, the pasting efficiency, the permeability and the bonding performance are improved, the substance is sulfonated through sulfamic acid, the solubility is improved, the flowing performance is improved, the methylation treatment is carried out through formaldehyde, and finally the lignin graft polymer is mixed with starch and epoxy chloropropane, and then the crosslinking reaction is carried out in the alkaline solution, so that the chemical stability, the pasting performance and the pasting efficiency are enhanced. The invention solves the problems of poor permeability and low pasting rate of the printing paste at present.)

1. A preparation method of printing paste is characterized by comprising the following steps:

(1) ball-milling the pretreated lignin and the compound according to a mass ratio of 4-6: 10-16, collecting ball-milled substances, and taking 130-150 parts of compound solution, 50-60 parts of ball-milled substances, 20-25 parts of acetone, 13-15 parts of additives, 7-9 parts of reducing agent and 3-6 parts of initiator according to parts by weight;

(2) firstly, placing the composite solution, the ball mill and a reducing agent into a reaction kettle, carrying out nitrogen protection, stirring, keeping the temperature at 50-55 ℃, adding an additive, heating, adding an initiator, carrying out stirring reaction, adding acetone, and standing;

(3) after standing, discharging, spray drying, washing with ethanol, drying, collecting the dried product, performing ultrasonic oscillation on the dried product, an auxiliary agent and water according to the mass ratio of 3-6: 1:15, heating to 90-100 ℃, stirring, adding a synergist accounting for 20-40% of the mass of the auxiliary agent, cooling to 60-70 ℃, and mixing;

(4) after mixing, spray drying, collecting spray-dried substances, stirring and heating the spray-dried substances, starch, epoxy chloropropane and sodium hydroxide solution according to the mass ratio of 8-13: 4: 2-4: 26, cooling, freeze drying, washing and drying to obtain the printing paste.

2. The printing paste preparation method according to claim 1, wherein the pretreatment lignin in the step (1) is prepared by mixing lignin, a surfactant and a sodium hydroxide solution in a mass ratio of 1:0.2: 4-6, stirring, filtering, adjusting the pH of the filtrate to 2-3, heating, standing, filtering, washing, drying, and collecting the dried product to obtain the pretreatment lignin.

3. The method for preparing printing paste according to claim 2, wherein the surfactant is any one of sodium dodecylbenzenesulfonate and sodium dodecylsulfate.

4. The preparation method of the printing paste according to claim 1, wherein the compound in the step (1) is prepared by mixing cyclodextrin and sodium alginate according to a mass ratio of 2: 7-10.

5. The method for preparing printing paste according to claim 1, wherein the composite solution is prepared by mixing dimethyl sulfoxide and sodium hydroxide solution in a volume ratio of 4: 6-8.

6. The method for preparing printing paste according to claim 1, wherein the additive is prepared by stirring toluene diisocyanate and acrylic acid in a mass ratio of 3: 2-6.

7. The method for preparing printing paste according to claim 1, wherein the reducing agent is sodium thiosulfate and oxalic acid mixed in a mass ratio of 13: 1.

8. The method of producing printing paste according to claim 1, wherein the initiator is any one of sodium persulfate, ammonium persulfate, and potassium persulfate.

9. The process for the preparation of printing paste according to claim 1, wherein the adjuvant in step (3) is sulfamic acid.

10. The process for the preparation of printing paste according to claim 1, wherein the synergist in step (3) is formaldehyde.

Technical Field

The invention belongs to the technical field of textile printing and dyeing, and particularly relates to a preparation method of printing paste.

Background

With the overall improvement of the economic level in the world, the demands of people on clothes, textiles and the like tend to be more personalized and diversified. Compared with the dyed fabric, the printed fabric has the advantages that the color and the patterns are changed, so that the printed fabric has strong artistic effect and aesthetic feeling, and the humanized requirement of people is greatly met. With current printing technology, both roller printing, screen printing and ink-jet printing involve printing pastes. The printing paste is a high molecular compound which can play a thickening role when added into printing paste. The printing effect of the paste printing is closely related to the printed fabric, the printing method and the printing paste consisting of the paste, the dye and the auxiliary agent. The printing paste is the most important factor in determining the printing quality, since it controls the rheology of the printing paste and the penetration and migration of the printing paste. Before the printing paste is added into the printing paste, the printing paste is generally a hydrophilic high molecular thick colloidal solution which is dissolved in water or can be fully swelled and dispersed in water, or an oil/water type or water/oil type emulsified paste. When the dye is blended into the printing paste, one part of the dye is dissolved in water, and the other part of the dye is dissolved, absorbed or dispersed in the printing paste. The printing paste is the main component of printing colour paste, and is used as carrier and medium of dye and adjuvant in the printing process, and it can determine printing running performance, colour-giving quantity of dye, fineness and clearness of pattern contour, etc. In summary, the quality of the printed product depends to a large extent on the quality of the printing paste, the properties of which directly affect the quality and cost of the final product.

At present, the printing paste used for the fabric mainly comprises natural paste; and synthesizing paste and composite paste. The natural paste mainly comprises sodium alginate, modified starch or cellulose, guar gum, tamarind gum and the like. The synthesized paste mainly comprises an acrylic ester thickener, a polyether ester thickener and the like. The composite paste mainly comprises a composite of a natural paste and a synthetic thickener, a composite of an inorganic thickener (clay, montmorillonite or sepiolite) and the natural paste, a composite of an emulsifying paste and the natural paste, a composite of the emulsifying paste and the synthetic thickener and the like. Generally, printing pastes can be different according to different types of printing fibers, different types of dyes, different printing equipment and different specific printing operations; also printing pastes have for a long time mainly used starch pastes. Although it has the advantages of low price and rich color, the paste-making and pulp-boiling time is long, the energy consumption is large, the defects of staining, dust and the like are easily generated during washing, and the permeation effect and the hand feeling are poor. Patent CN1095120 proposes an inorganic printing paste which is prepared by using montmorillonite powder as a main raw material (95-99%) and adding a small amount of instant sodium carboxymethylcellulose (1-5%) into the montmorillonite powder to form a powder, and has the advantages of simple production process and low cost, but the patent does not provide an implementation method for applying the inorganic printing paste to printing of towels and velvet fabrics. Patent CN102296468A provides a transfer printing paste for natural fiber velveteen and a production method thereof. The printing paste is formed by combining sodium carboxymethyl starch raw paste and polyvinyl alcohol PVA raw paste. However, the printing paste is only used for transfer printing of velveteen fabrics, the limitation is obvious, and the waste water of the printing paste contains a large amount of PVA, so that the printing paste is not easy to biodegrade, and the difficulty in sewage treatment is increased. Seed gum pastes such as guar gum and locust bean gum are mostly used in foreign technologically advanced countries, especially in silk broadcloth printing. In order to overcome the defects that the seed gelatine powder cannot be quickly swelled and hydrated, has low dissolving speed, high content of water-insoluble substances, difficult control of viscosity, is easy to decompose by microorganisms and cannot be stored for a long time and the like, the seed gelatine powder needs to be chemically modified, and the physicochemical characteristics of the seed gelatine powder are changed, so that the seed gelatine powder has the characteristics of good printing performance, good permeability, good leveling property of printing block surfaces, high pasting rate and the like.

Disclosure of Invention

The technical problems to be solved by the invention are as follows: aiming at the problems of poor permeability and low pasting rate of the current printing paste, the invention provides a preparation method of the printing paste.

In order to solve the technical problems, the invention adopts the following technical scheme:

a preparation method of printing paste comprises the following steps:

(1) ball-milling the pretreated lignin and the compound according to a mass ratio of 4-6: 10-16, collecting ball-milled substances, and taking 130-150 parts of compound solution, 50-60 parts of ball-milled substances, 20-25 parts of acetone, 13-15 parts of additives, 7-9 parts of reducing agent and 3-6 parts of initiator according to parts by weight;

(2) firstly, placing the composite solution, the ball mill and a reducing agent into a reaction kettle, carrying out nitrogen protection, stirring, keeping the temperature at 50-55 ℃, adding an additive, heating, adding an initiator, carrying out stirring reaction, adding acetone, and standing;

(3) after standing, discharging, spray drying, washing with ethanol, drying, collecting the dried product, performing ultrasonic oscillation on the dried product, an auxiliary agent and water according to the mass ratio of 3-6: 1:15, heating to 90-100 ℃, stirring, adding a synergist accounting for 20-40% of the mass of the auxiliary agent, cooling to 60-70 ℃, and mixing;

(4) after mixing, spray drying, collecting spray-dried substances, stirring and heating the spray-dried substances, starch, epoxy chloropropane and sodium hydroxide solution according to the mass ratio of 8-13: 4: 2-4: 26, cooling, freeze drying, washing and drying to obtain the printing paste.

The preparation method of the pretreated lignin in the step (1) comprises the steps of mixing lignin, a surfactant and a sodium hydroxide solution according to the mass ratio of 1:0.2: 4-6, stirring, filtering, adjusting the pH of the filtrate to 2-3, heating, standing, filtering, washing, drying, and collecting the dried substance to obtain the pretreated lignin.

The surfactant is any one of sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.

The compound in the step (1) is formed by mixing cyclodextrin and sodium alginate according to the mass ratio of 2: 7-10.

The composite solution is prepared by mixing dimethyl sulfoxide and sodium hydroxide solution according to a volume ratio of 4: 6-8.

The additive is prepared by stirring toluene diisocyanate and acrylic acid according to a mass ratio of 3: 2-6.

The reducing agent is formed by mixing sodium thiosulfate and oxalic acid according to the mass ratio of 13: 1.

The initiator is any one of sodium persulfate, ammonium persulfate and potassium persulfate.

The adjuvant in the step (3) is sulfamic acid.

The synergist in the step (3) is formaldehyde.

Compared with other methods, the method has the beneficial technical effects that:

the invention firstly alkalifies lignin by alkaline solution, adds surfactant to enhance activity, then mixes the lignin with cyclodextrin and sodium alginate, reacts with additive under the action of reducing agent and initiator in the environment of composite solution, reacts with acrylic acid in the additive under alkaline environment to form sodium acrylate, polymerizes under the action of initiator to form alkaline lignin graft polymer, and partially wraps the sodium alginate to improve paste forming efficiency, permeability and binding performance, and then carries out sulfonation treatment on substances in the additive by sulfamic acid to increase solubility and fluidity, carries out methylation treatment by formaldehyde, finally mixes the lignin with starch and epoxy chloropropane, carries out cross-linking reaction in alkaline solution to enhance chemical stability and paste removing performance, the paste forming efficiency is enhanced.

Detailed Description

The preparation method of the pretreated lignin comprises the steps of mixing lignin, a surfactant and 1.6mol/L sodium hydroxide solution according to the mass ratio of 1:0.2: 4-6, stirring for 2 hours, filtering, adjusting the pH of the filtrate to 2-3, heating to 95 ℃, standing for 6 hours, filtering, washing with ethanol, drying, and collecting the dried substance to obtain the pretreated lignin.

The surfactant is any one of sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.

The compound is formed by mixing cyclodextrin and sodium alginate according to the mass ratio of 2: 7-10.

The composite solution is prepared by mixing dimethyl sulfoxide and 1.3mol/L sodium hydroxide solution according to a volume ratio of 4: 6-8.

The additive is prepared by stirring toluene diisocyanate and acrylic acid according to a mass ratio of 3: 2-6.

The reducing agent is formed by mixing sodium thiosulfate and oxalic acid according to the mass ratio of 13: 1.

The initiator is any one of sodium persulfate, ammonium persulfate and potassium persulfate.

The adjuvant is sulfamic acid.

The synergist is formaldehyde.

A preparation method of printing paste comprises the following steps:

(1) ball-milling the pretreated lignin and the compound at a mass ratio of 4-6: 10-16 at 800r/min for 20min, collecting ball-milled substances, and taking 130-150 parts of compound solution, 50-60 parts of ball-milled substances, 20-25 parts of acetone, 13-15 parts of additives, 7-9 parts of reducing agent and 3-6 parts of initiator according to parts by weight;

(2) firstly, placing the composite solution, the ball mill and a reducing agent into a reaction kettle, stirring for 5 hours at 500r/min under the protection of nitrogen, keeping the temperature at 50-55 ℃, adding an additive, heating to 90-100 ℃, adding an initiator, stirring for reaction for 7-9 hours, adding acetone, and standing for 6 hours;

(3) after standing, discharging, spray drying, washing with ethanol, drying, collecting the dried product, performing ultrasonic oscillation on the dried product, an auxiliary agent and water according to the mass ratio of 3-6: 1:15 for 30min, heating to 90-100 ℃, stirring for 5h, adding a synergist accounting for 20-40% of the mass of the auxiliary agent, cooling to 60-70 ℃, and mixing for 2h at 600 r/min;

(4) after mixing, spray drying, collecting spray-dried substances, heating the spray-dried substances, starch, epoxy chloropropane and 1.7mol/L sodium hydroxide solution according to the mass ratio of 8-13: 4: 2-4: 26 to 80 ℃, stirring for 5 hours at 500r/min, cooling to room temperature, freeze drying, washing with ethanol, and drying to obtain the printing paste.