Low-alkali or alkali-free active bright-blue dye and preparation method thereof

A technology of reactive brilliant blue and dyes, which is applied in the direction of reactive dyes, azo dyes, organic dyes, etc., can solve the problems of high energy consumption, labor consumption, and waste water, and achieve the reduction of waste water discharge, energy saving, and good dryness. The effect of wet fastness

Inactive Publication Date: 2015-02-25

ZHEJIANG YIDE CHEM

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AI-Extracted Technical Summary

Problems solved by technology

[0003] The chlorine on the active group "chlorotriazine" in the traditional KE or HE reactive dyes is open. The traditional blending and interweaving dyeing process is po...

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Method used

Embodiment 2: 100g cotton cloth, a kind of low-alkali obtained by embodiment 1 or alkali-free type reactive brilliant blue dye, by fabric weight 2%, containing 60g/l Yuan Mingfen, bath ratio are 20:1 In the dye bath, absorb at 60°C for 30 minutes, add s...

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Abstract

The invention relates to the field of active dye in the novel technology and especially relates to low-alkali or alkali-free active bright-blue dye and a preparation method thereof. The invention provides the low-alkali or alkali-free active bright-blue dye shown in the formula (1), and in the formula (1), M represents hydrogen or alkali metal. In dyeing, the low-alkali or alkali-free active bright-blue dye can be crosslinked and fixed to cotton fibers only by use of 1-3g/l of an alkali agent and even, the low-alkali or alkali-free active bright-blue dye can be crosslinked and fixed to the cotton fibers under the condition of dyeing bath pH of 7 and no alkali agent. The preparation method is a novel technology completely different from the traditional technology and is especially suitable for blended fabric dyeing. The low-alkali or alkali-free active bright-blue dye and the cotton fibers are bonded by covalent bonds and thus dry and wet fastness, solarization fastness and washing fastness are stable and good. Separated picolinic acid is a vitamin and has small influence on the environment.

Application Domain

Reactive dyes

Technology Topic

DyeingFormic acid +11

Image

Examples

Experimental program(3)

Example Embodiment

[0044] Example 1: Preparation of reactive brilliant blue of formula (1-1).

[0045] A, a shrinkage reaction

[0046] 8g of cyanuric chloride, 30g of water, 100g of ice, 1g of dispersant, and beating for 1 hour at 0-3°C, add 2.4-disulfonic acid aniline solution (pre-configuration: 10g of 2.4-disulfonic acid aniline + 100g of water, add soda ash dry powder Adjust pH=5-7 by 3g, stir and dissolve to clear), the feeding speed shall be controlled as pH≤5.0. After the addition, keep at 5-15℃ and react, then slowly add 5g baking soda to adjust pH=5-7, and the reaction will reach the end ( 9-10 hours).

[0047] B, dicondensation reaction

[0048] Once the end of the reduction is reached, add 25g of Reactive Blue 198 color base to the first reduction solution, adjust the pH to 7-9 with 3g of soda ash, after the addition, heat up to 30-50℃ for reaction, and use 4g of soda ash to keep the pH during the reaction =7-9, until the end of the reaction (reaction for 1-2 hours).

[0049] E. Triple shrinkage reaction

[0050] 6g dry powder of niacin was directly added to the coupling solution, and after stirring for 10 minutes, the temperature was directly raised to 80-95°C, and the pH was maintained at 4-7 with 8g baking soda. Control the reaction to the end (8-10 hours of reaction).

[0051] F, steam drying

[0052] After reaching the end point, it was directly dried with steam to obtain 73 g of the reactive brilliant blue dye of formula (1-1).

[0053] G. The raw materials used and their corresponding structural formulas are shown in Table 1.

[0054] Table 1

[0055]

[0056]

Example Embodiment

[0057] Example 2: Preparation of reactive brilliant blue of formula (1-2).

[0058] A, a shrinkage reaction

[0059] 8g of cyanuric chloride, 30g of water, 100g of ice, 1g of dispersant, and beating for 1 hour at 0-3°C, add 2.4-disulfonic acid aniline solution (pre-configuration: 10g of 2.4-disulfonic acid aniline + 100g of water, add soda ash dry powder Adjust pH=5-7 by 3g, stir and dissolve to clear), the feeding speed shall be controlled as pH≤5.0. After the addition, keep at 5-15℃ and react, then slowly add 5g baking soda to adjust pH=5-7, and the reaction will reach the end ( 9-10 hours).

[0060] B, dicondensation reaction

[0061] Once the end of the reduction is reached, add 25g of Reactive Blue 198 color base to the first reduction solution, adjust the pH to 7-9 with 3g of soda ash, after the addition, heat up to 30-50℃ for reaction, and use 4g of soda ash to keep the pH during the reaction =7-9, until the end of the reaction (reaction for 1-2 hours).

[0062] E. Triple shrinkage reaction

[0063] 6g of niacin or isonicotinic acid dry powder is directly added to the coupling solution, after stirring for 10 minutes, the temperature is directly raised to 80-95°C, and the pH is maintained at 4-7 with 8g of baking soda. Control the reaction to the end (8-10 hours of reaction).

[0064] F, steam drying

[0065] After the end point is reached, it is directly dried with steam to obtain 73 g of formula (1-2) reactive brilliant blue dye.

[0066] G. The raw materials used and their corresponding structural formulas are shown in Table 2

[0067] Table 2

[0068]

Example Embodiment

[0069] Example 3: Several formulas were selected according to the characteristics of superior application performance, etc., as shown in Table 3. The application properties of the reactive dyes prepared in the examples of the present invention are shown in Table 4 and Table 5 below.

[0070] table 3

[0071] Serial number

[0072] Each reactive dye composition in Table 1 above is dry powder mixed in a mixing tank, or dissolved together and spray dried. There are other reactive dye compositions that are not listed one by one, but are included in the present invention.

[0073] Example 2: 100g cotton cloth, a low-alkali or alkali-free reactive brilliant blue dye obtained according to Example 1, 2% by weight of the fabric, in a dye bath containing 60g/l sodium sulfate and a bath ratio of 20:1 In the medium, adsorb for 30min at 60℃, add soda ash (dosage 15-20g/l) to fix for 45min. The dyed fabric is washed, soaped and dried. The obtained dyed cotton cloth has uniform color and satisfactory fastness to sunlight and moisture treatment. See Table 4 for specific performance.

[0074] Table 4

[0075]

[0076] table 5

[0077]

[0078]

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Description & Claims & Application Information

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