KR101007979B1 - Manufacturing method for discharge printing agent and a new discharge printing agent proudced by the manufacturing method - Google Patents

Abstract

The present invention relates to a method for preparing a printing agent and a new printing agent prepared by the method, comprising the steps of: a) heating poly oxyethylene glycol to 75 to 85 ° C; (b) adding citric acid or maleic acid to the elevated polyoxyethylene glycol and maintaining 75 to 85 ° C. until dissolved; (c) adding dicyandiamide or melamine to the resultant of step (b) and maintaining 55 to 65 ° C. until dissolved; (d) adding stannous chloride to the resultant of step (c) and maintaining 40 to 50 ° C until dissolved; And (e) adding and dissolving triethanolamine, trichlorobenzene, and fluorescent brightener to the resultant of step (d); 12 weight percent of dicyandiamide or melamine; 8% by weight poly oxyethylene glycol; 8% by weight triethanolamine; 5 weight percent trichlorobenzene; 16.5% citric acid or maleic acid; And it provides a flame retardant comprising 0.5% by weight of a fluorescent brightener. According to the present invention, even if stored for a long period of time, there is no occurrence of stones or deterioration in the ability of printing, and the concentration of the first-chloride chloride is two times higher than that of the conventional printing agent. In addition, as a result of using the flame retardant according to the present invention, the degree of flame retardancy was improved by about 1 degree in gray scale (grey scale) compared to the existing flame retardant, and the light fastness of the moistened portion was improved by level 1 or more.

Description

Manufacturing method for a printing agent and a new printing agent produced by the manufacturing method {proud manufacturing by the manufacturing method}

The present invention relates to a method for producing a printing agent, and a new printing agent prepared by the method, in particular, increasing the content of first salt without using water (water) and causing stones even when stored for a long period of time. The present invention relates to a new flame retardant without deterioration and a manufacturing method capable of manufacturing the same.

Phosphorus dyeing of textile crops is to invent a stamped part by stamping a printing agent in which a dyeing agent is added to a fabric which has been dyed with a bottom. As a method of removing the color of the bottom dyed fabric by using a printing agent, there are white printing, duplex printing, coloring printing, and the like. According to the type of the printing agent, there are oxidation and reduction printing.

A fluorophore refers to a chemical composition that removes dyes dyeing on fabrics by applying oxidation and reduction of chemicals. The propellants which have been used in the oxidative invention until now are potassium chloride, potassium permanganese, septic salt, erythritis, potassium dichromate, bleach powder, etc. The propellants which have been used for reduction invention are zinc powder, sodium hydrogen sulfite, sodium sulfite, Stannous chloride, sodium hydrosulfite, and long gallet. However, even when such a composition is used as a propellant, the type and content of each component have a great influence on the result of the prophylaxis due to the characteristics of each component of the propellant or the interaction with each other.

In particular, in the printing process, not only the influence of the printing agent, but also the influence of the materials such as the type of fabric, dyes, dyes, pharmaceuticals, and mechanical tolerances of the printing machine, the dryer, the steamer, the washing machine, the featherer, etc. Occupies.

Among these, the type and content of each component of the printing agent can be said to have an almost absolute effect on the printing process. Therefore, in order to satisfy the quality of the printed fabric, the development of the printing agent is continued, but it does not show satisfactory performance.

In particular, since the conventional flame retardant uses water, long-term tube stones occur and the ability to reduce the repellency has a problem that a desired degree of whiteness cannot be obtained even when the amount of the repellent is increased.

Accordingly, the problem to be solved by the present invention is to provide a new flame retardant and a method for producing the same that does not occur the above-described problem. That is, an object of the present invention is to provide a flame retardant and a method for producing the same, which are capable of improving whiteness and daylight fastness as a result of the spontaneity, since the stones do not occur even if stored for a long period of time, and the immunity does not decrease.

The present invention to achieve the above technical problem,

(a) heating poly oxyethylene glycol to 75 to 85 ° C;

(b) adding citric acid or maleic acid to the elevated polyoxyethylene glycol and maintaining 75 to 85 ° C. until dissolved;

(c) adding dicyandiamide or melamine to the resultant of step (b) and maintaining 55 to 65 ° C. until dissolved;

(d) adding stannous chloride to the resultant of step (c) and maintaining 40 to 50 ° C until dissolved; And

(e) It provides a method for producing a flame retardant comprising the step of dissolving the triethanolamine (triethanolamine), trichlorobenzene (triclorobenzen) and fluorescent brightener (fluorescent brightener) to the result of step (d).

In the method for preparing a flame retardant according to the present invention as described above, the weight average molecular weight of the polyoxyethylene glycol is preferably 300 to 400.

In addition, the present invention to achieve the above other technical problem,

(a) heating poly oxyethylene glycol to 75 to 85 ° C;

(b) adding citric acid or maleic acid to the elevated polyoxyethylene glycol and maintaining 75 to 85 ° C. until dissolved;

(c) adding dicyandiamide or melamine to the resultant of step (b) and maintaining 55 to 65 ° C. until dissolved;

(d) adding stannous chloride to the resultant of step (c) and maintaining 40 to 50 ° C until dissolved; And

(e) triethanolamine, trichlorobenzene, and fluorescent brightener are added to the resultant of step (d) to dissolve it.

50% by weight of stannous chloride;

12 weight percent of dicyandiamide or melamine;

8% by weight poly oxyethylene glycol;

8% by weight triethanolamine;

5 weight percent trichlorobenzene;

16.5% citric acid or maleic acid; And

0.5% by weight of fluorescent varnish

It provides a propellant comprising.

According to the method of manufacturing a flame retardant according to the present invention as described above, water is not used in the production of the flame retardant according to the appropriate temperature conditions, and the concentration of first-chloride chloride can be increased almost twice as compared to the conventional flame retardant, The propellant does not have stones or deterioration in the ability to print even if stored for a long period of time, and the concentration of first-chloride chloride is twice that of the conventional propellant, so it is easy to use and convenient to store and transport. In addition, as a result of using the flame retardant according to the present invention, the degree of flame retardancy was improved by about 1 degree in gray scale (grey scale) compared to the existing flame retardant, and the light fastness of the moistened portion was improved by level 1 or more.

Hereinafter, specific contents for the practice of the present invention will be described.

According to the present invention, when the amount of the first salt chloride is about 25% by weight, the content of the first salt chloride is increased by about two times, and the manufacturing process of the printing agent is stored for a long time without using water. This invention solves the problem of the absent stone which arises and the fall of printing force.

In order to solve the above, the inventors of the present invention use poly oxyethylene glycol as a basic solvent and increase the temperature of the poly oxyethylene glycol, and then gradually lower the temperature so that the optimum solubility can be exerted at each temperature. The propellant was prepared by adding and dissolving possible ingredients.

Looking at the manufacturing method according to the present invention in detail.

First, the polyoxyethylene glycol (poly oxyethylene glycol) is heated to 75 ~ 85 ℃ and while maintaining this temperature is added to citric acid (citric acid) or maleic acid (maleic acid) to the polyoxyethylene glycol completely dissolved. When melting is complete, it becomes transparent and can be grasped by the naked eye. It is important to keep the temperature between 75 and 85 ° C. until dissolution is maintained completely.

Subsequently, when the temperature of the solution in which citric acid or maleic acid is dissolved in polyoxyethylene glycol is 55 to 65 ° C., dicyandiamide or melamine is added, followed by 55 to 65 ° C. It is a complete dissolution of dicyandiamide or melamine while maintaining. At this time, since the state of the solution becomes transparent after being dissolved, whether or not it is completely dissolved can be grasped visually. In addition, when dissolving dicyandiamide or melamine, be careful about the exothermic reaction when dissolving, which can cause the temperature to exceed 55 ~ 65 ℃, allowing the coolant to flow around the melting vessel to maintain the temperature. shall.

Next, after dissolution of dicyandiamide or melamine is completed, wait for the temperature of the solution to reach 40 to 50 ° C. Then, add 1st chloride and maintain 40 to 50 ° C. To dissolve it. At this time, since the dissolution of the first salt chloride is an endothermic reaction, the temperature may drop below 40 ° C., so it is important to maintain the temperature while appropriately heating.

Subsequently, when dissolution of the first salt is completed, the remaining ingredients that can be dissolved irrespective of temperature are added to triethanolamine, trichlorobenzene, and fluorescent brightener to dissolve the propellant according to the present invention. The manufacture of is completed.

In the preparation of the flame retardant according to the present invention as described above, in the case of the polyoxyethylene glycol, using a weight average molecular weight of 300 to 400 showed an optimal effect to achieve the object of the present invention, 1500 In the case of to 4,000 was shown a problem that can not achieve the purpose.

As a result of the production according to the method for producing a flame retardant according to the present invention as described above was able to increase the content of the first stone chloride up to about 50% by weight, the composition of the flame retardant for the optimal effect,

50% by weight of stannous chloride;

12 weight percent of dicyandiamide or melamine;

8% by weight poly oxyethylene glycol;

8% by weight triethanolamine;

5 weight percent trichlorobenzene;

16.5% citric acid or maleic acid; And

0.5% by weight of fluorescent varnish

It was to include.

Hereinafter, the effects of the flame retardant according to the present flame retardation will be described through experiments through the polyester fiber repellent processing.

<Examples>

The composition of the flame retardant is 50% by weight of stannous chloride, 12% by weight of dicyandiamide, 8% by weight of polyoxyethylene glycol, 8% by weight of triethanolamine, 5% by weight of trichlorobenzene, 16.5% by weight of citric acid and 0.5% by weight of fluorescent brightener. 10 kg of this print was prepared.

First, polyoxyethylene glycol (weight average molecular weight 400, CAS No 25322-68-3) is placed in a container and warmed up to 80 ° C., and then citric acid (CAS No 77-92-) is maintained in polyoxyethylene glycol while maintaining this temperature. 9) was added and dissolved completely until clear. The dissolution time was about 2 hours.

Subsequently, the solution was waited until the temperature dropped to 60 ° C., and then dicyandiamide (CAS No 461-58-5) was added thereto, followed by complete dissolution with stirring until clear. At this time, 60 ℃ was maintained while dissolving, and dissolution of dicyandiamide was an exothermic reaction, so that the cooling water was kept in the surrounding water of the container. The dissolution time took about 4 hours.

After dissolution of dicyandiamide is complete, wait for the temperature of the solution to reach 50 ° C, and then dissolve the ferrous chloride while adding 50 ° C (CAS No 7772-99-8) and maintaining 50 ° C. . At this time, since the dissolution of the first salt chloride is an endothermic reaction, when the temperature drops below 50 ° C., the dissolution is performed while placing a heater under the container and warming it. The dissolution time took about 4 hours.

Subsequently, when dissolution of the first salt is completed, triethanolamine (CAS No 102-72-6), trichlorobenzene (CAS No 120-82-1) and fluorescent brightener 199 Fluorescent brightener 199, trade name Palanil White R) was added to dissolve to complete the preparation of the propellant.

<Test Example 1>

Working process for testing

1) Inflammation

Preparation of Polyester Fabric Dyed with Wig Dye

Printing Agent-> Steam-> Flushing-> Drying

2) Flameproof

Printing agent-> Drying-> Wig dye Padding-> Steaming-> Flushing-> Drying

Wig dye padding uses O company discharge Black 18%

The amount of conventional processed stone dispersant in use and the dispersant prepared in Example (see Table 1)

One 2 3 4 5 6 7 8 Conventional Plaster 20 30 40 50 - - - - EXAMPLE Plasters - - - - 10 15 20 25 Horyo (13%) 80 70 60 50 90 85 80 75 Totel 100 100 100 100 100 100 100 100

result

1) Whiteness comparison (Grey scale judgment, Table 2, Judgment unit; grade)

Propellant
Room One 2 3 4 5 6 7 8 Black Knitted Print One 2 3 3 2 2-3 3 3-4 Brown Fabric Printed One 2-3 3 3 2 2-3 3 3-4 Black Flame Retardant 1-2 2-3 3-4 3-4 2 3-4 4 4

2) Daylight fastness comparison

Dyeing fastness to KSK 0218 xenon arc (Table 3, Judgment Unit: Grade)

Propellant
Room 3 7 Black Knitted Print 3 3-4 Brown Fabric Printed 3 3-4 Black Flame Retardant 3-4 4

As shown in Table 2 and Table 3, the amount of the propellant was reduced in half compared to the conventional propellant, but it can be seen that the nominal effect on the whiteness and the light fastness of the propellant increased by 2 times. .

<Test Example 2>

The conventional ignition agent containing the first salt chloride and the ignition agent according to the present invention prepared in the above embodiment was stored for about 6 months, and whether or not stones were observed was observed every 15 days. In the case of the conventional ignition agent, about 45 days Although the stones were observed to the extent, the stones were not observed even after a period of 6 months in the case of the propellant according to the present invention prepared in the above examples.

As described above, according to the present invention, it was confirmed that the problem of absence due to long-term storage and the problem of lowering the printing force can be solved.

Claims (3)

(a) heating poly oxyethylene glycol to 75 to 85 ° C; (b) adding citric acid or maleic acid to the elevated polyoxyethylene glycol and maintaining 75 to 85 ° C. until dissolved; (c) adding dicyandiamide or melamine to the resultant of step (b) and maintaining 55 to 65 ° C. until dissolved; (d) adding stannous chloride to the resultant of step (c) and maintaining 40 to 50 ° C until dissolved; And (e) a method of producing a printing agent comprising the step of adding and dissolving triethanolamine, trichlorobenzene, and fluorescent brightener to the resultant of step (d). The method of claim 1, The weight average molecular weight of the polyoxyethylene glycol is 300 to 400, characterized in that the method for producing a flame retardant composition. (a) heating poly oxyethylene glycol to 75 to 85 ° C; (b) adding citric acid or maleic acid to the elevated polyoxyethylene glycol and maintaining 75 to 85 ° C. until dissolved; (c) adding dicyandiamide or melamine to the resultant of step (b) and maintaining 55 to 65 ° C. until dissolved; (d) adding stannous chloride to the resultant of step (c) and maintaining 40 to 50 ° C until dissolved; And (e) triethanolamine, trichlorobenzene, and fluorescent brightener are added to the resultant of step (d) to dissolve it. 50% by weight of stannous chloride; 12 weight percent of dicyandiamide or melamine; 8% by weight poly oxyethylene glycol; 8% by weight triethanolamine; 5 weight percent trichlorobenzene; 16.5% citric acid or maleic acid; And 0.5% by weight of fluorescent varnish Inflammatory agent comprising a.