阅读说明：本技术 一种羊绒漂白活化剂的制备方法 (A kind of preparation method of cashmere bleach-activating ) 是由 罗峰 于 2019-08-06 设计创作，主要内容包括：本发明涉及一种羊绒漂白活化剂的制备方法,属于纺织技术领域。本发明在使用过程中,首先利用活化剂中的超支化聚合物离子物质可以有效的与色素进行结合,破坏色素与色素直接的不饱和键,从而破坏色素的共轭系统,增加过氧化氢的漂白效果,其次通过其中的钛硅颗粒催化双氧水的分解,增加了分解率,并且通过钛硅颗粒的作用可以有效催化混合料中的叔丁醇、环己酮与辅助剂为氨水进行反应,产生环己酮肟,通过反应过程可以提高过氧化氢的分解性能,提高漂白效果,另外环己酮肟可以与过氧化氢进行反应,产生更好的氧化漂白效果,增强漂白性能。本发明解决了目前羊绒漂白过程中过氧化氢的漂白效率低的问题。(The present invention relates to a kind of preparation methods of cashmere bleach-activating, belong to textile technology field.The present invention is in use, it can be effectively combined with pigment first with the dissaving polymer ionic species in activator, destroy pigment and the direct unsaturated bond of pigment, to chromatophagous conjugated system, increase the bleaching effect of hydrogen peroxide, secondly by the decomposition of titanium silicon particle therein catalysis hydrogen peroxide, increase resolution ratio, and it can the tert-butyl alcohol effectively in catalytic mixing material by the effect of titanium silicon particle, cyclohexanone is that ammonium hydroxide is reacted with adjuvant, generate cyclohexanone oxime, the decomposability of hydrogen peroxide can be improved by reaction process, improve bleaching effect, in addition cyclohexanone oxime can be reacted with hydrogen peroxide, generate better oxidation bleaching effect, enhance bleachability.The present invention solves the problems, such as that the bleaching efficiency of hydrogen peroxide in current cashmere bleaching process is low.)

1. a kind of preparation method of cashmere bleach-activating, which is characterized in that the preparation method includes the following steps:

(1) it takes silica solution, surfactant and ethanol solution 7~9:1:20 in mass ratio to carry out ultrasonic vibration, is put into reaction kettle In, the butyl titanate of the template of silica solution quality 20~25%, silica solution quality 20~25% is added, 50~60 DEG C into Row preheating；

(2) after preheating, nitrogen protection is added the ethanol amine of silica solution quality 50~55%, is warming up to 90~95 DEG C, stirs It mixes, is cooled to 45~50 DEG C, stand, discharge, dried object is collected in spray drying；

(3) according to parts by weight, take 160~180 parts of mixed solvents, 40~50 parts of dried objects, 12~14 parts of resorcinols, 11~ 13 parts of trimellitic anhydrides, 10~13 parts of functives, 4~10 parts of auxiliary agents, 1~3 part of additive；

(4) mixed solvent, dried object, resorcinol, trimellitic anhydride and auxiliary agent are put into reaction kettle first, nitrogen protection, 125~130 DEG C are warming up to, is stirred to react, is cooled to 105~110 DEG C, adds functive and additive, is stirred, it is cooling, out Material, material out is mixed with ether 4:7~9 in mass ratio, is stood, and filter residue is collected in filtering, is washed, dry, collects dried object A；

(5) dried object A, mixture, adjuvant and stabilizer 7~9:3:1 in mass ratio~3:0.2 are uniformly mixed to get sheep Suede bleach-activating.

2. the preparation method of cashmere bleach-activating according to claim 1, which is characterized in that surface in the step (1) Activating agent are as follows: sodium cocoyl methyl sodium taurocholate, lauroylamidopropyl betaine, any one in Coconut Fatty Acid Monoethanolamide Kind.

3. the preparation method of cashmere bleach-activating according to claim 1, which is characterized in that template in the step (1) Agent is dodecyl sodium sulfate, cetyl trimethylammonium bromide 1:8~10 in mass ratio are stirred to get template.

4. the preparation method of cashmere bleach-activating according to claim 1, which is characterized in that the functive is N- methyl Bromo- 4- nitroimidazole 9:2~4 in mass ratio imidazoles, 2- mix.

5. the preparation method of cashmere bleach-activating according to claim 1, which is characterized in that the auxiliary agent is epoxy chloropropionate Alkane, acrylamide 6~9:2 in mass ratio are mixed.

6. the preparation method of cashmere bleach-activating according to claim 1, which is characterized in that the additive be urea, Any one in ammonium hydrogen carbonate, sodium bicarbonate.

7. the preparation method of cashmere bleach-activating according to claim 1, which is characterized in that the mixed solvent is ethyl alcohol 7:1~3 mix by volume for solution, N,N-dimethylformamide.

8. the preparation method of cashmere bleach-activating according to claim 1, which is characterized in that mixing in the step (5) Material is the tert-butyl alcohol, cyclohexanone 9:1~6 in mass ratio mix.

9. the preparation method of cashmere bleach-activating according to claim 1, which is characterized in that auxiliary in the step (5) Agent is that sodium acetate is mixed with ammonium hydroxide 1:10~13 in mass ratio.

10. the preparation method of cashmere bleach-activating according to claim 1, which is characterized in that stablize in the step (5) Agent is sodium dihydrogen phosphate.

Technical field

The present invention relates to a kind of preparation methods of cashmere bleach-activating, belong to textile technology field.

Background technique

Wool and cashmere fiber are one of earliest textile fibers of human use.The mankind probably the Neolithic Age just It has begun and uses.Moreover, they are very high-grade one of textile fibers.Since their fibre is with very more Excellent characteristic feel very abundant and there is elasticity for example, soft glossy, and have extraordinary comfortable and easy to wear Property etc., so their fibre is constantly subjected to the favor of consumer.Since wool is per se with color, although through bleaching Afterwards, color is removed, but for high-grade fabric, whiteness cannot still reach requirement；Purple cashmere is that black goat is produced Cashmere fiber is divided into darkviolet and two kinds of purple.Containing few green suede, white suede and red Down Fiber in purple Down Fiber；Because of purple sheep Suede per se with color it is deeper, the weaving finished product being process can only be natural colour either deeper color, so purple The application of suede is extremely restricted.So either wool fiber or cashmere fiber, require further to bleach and decoloration, Use demand can be reached.

Cashmere fiber is also designated as cashmere, refers to the under hair obtained from goat back, cashmere fiber be roughly divided into it is white, Green, red, purple four kinds of colors.Cashmere fiber feel is finer and smoother relative to wool fiber, smooth, warming, high resilience.Therefore cashmere Fiber is referred to as " soft gold ".This title also reflects the preciousness of cashmere fiber.In addition from yield, whole world Cashmere fiber The yield of dimension is about the 1% of production of wool.Shabri fiber therein is even more fewer and fewer, therefore cashmere decoloration just has very much It is necessary.

Currently, the widest oxidative bleaches of domestic and international application are hydrogen peroxide, hydrogen peroxide is commonly called as hydrogen peroxide, due to Hydrogen peroxide carries out oxidation bleaching and environmental issue is not present, and prospect is had an optimistic view of by numerous colourists.Due to wool and Cashmere fiber Dimension belongs to protein fibre, and the isoelectric point of wool and cashmere fiber is between 4.2~4.8, so if can be right under acid condition again Wool fiber is bleached and carries out the decoloration of cashmere fiber, then is greatly improved wool and cashmere fiber after treatment strong Power.But since in acid condition, the resolution ratio of hydrogen peroxide is relatively low, and bleaching power also decreases, to wool fiber Carry out bleaching and cashmere fiber decolourized after whiteness cannot reach the whiteness of requirement.

Summary of the invention

The technical problems to be solved by the invention: low for the bleaching efficiency of hydrogen peroxide in current cashmere bleaching process Problem, the present invention provides a kind of preparation methods of cashmere bleach-activating.

In order to solve the above technical problems, the present invention is using technical solution as described below:

A kind of preparation method of cashmere bleach-activating, the preparation method include the following steps:

(1) it takes silica solution, surfactant and ethanol solution 7~9:1:20 in mass ratio to carry out ultrasonic vibration, is put into reaction kettle In, the butyl titanate of the template of silica solution quality 20~25%, silica solution quality 20~25% is added, 50~60 DEG C into Row preheating；

(2) after preheating, nitrogen protection is added the ethanol amine of silica solution quality 50~55%, is warming up to 90~95 DEG C, stirs It mixes, is cooled to 45~50 DEG C, stand, discharge, dried object is collected in spray drying；

(3) according to parts by weight, take 160~180 parts of mixed solvents, 40~50 parts of dried objects, 12~14 parts of resorcinols, 11~ 13 parts of trimellitic anhydrides, 10~13 parts of functives, 4~10 parts of auxiliary agents, 1~3 part of additive；

(4) mixed solvent, dried object, resorcinol, trimellitic anhydride and auxiliary agent are put into reaction kettle first, nitrogen protection, 125~130 DEG C are warming up to, is stirred to react, is cooled to 105~110 DEG C, adds functive and additive, is stirred, it is cooling, out Material, material out is mixed with ether 4:7~9 in mass ratio, is stood, and filter residue is collected in filtering, is washed, dry, collects dried object A；

(5) dried object A, mixture, adjuvant and stabilizer 7~9:3:1 in mass ratio~3:0.2 are uniformly mixed to get sheep Suede bleach-activating.

Surfactant in the step (1) are as follows: sodium cocoyl methyl sodium taurocholate, lauroylamidopropyl betaine, coconut palm Any one in oleic monoethanolamide.

In the step (1) template be dodecyl sodium sulfate, cetyl trimethylammonium bromide 1:8 in mass ratio~ 10 are stirred to get template.

The functive is N- methylimidazole, bromo- 4- nitroimidazole 9:2~4 in mass ratio 2- mix.

The auxiliary agent is epoxychloropropane, acrylamide 6~9:2 in mass ratio is mixed.

The additive is urea, ammonium hydrogen carbonate, any one in sodium bicarbonate.

The mixed solvent is ethanol solution, 7:1~3 mix N,N-dimethylformamide by volume.

Mixture is the tert-butyl alcohol in the step (5), cyclohexanone 9:1~6 in mass ratio mix.

Adjuvant is that sodium acetate is mixed with ammonium hydroxide 1:10~13 in mass ratio in the step (5).

Stabilizer is sodium dihydrogen phosphate in the step (5).

The present invention is compared with other methods, and advantageous effects are:

(1) present invention using silica solution (wherein the dioxide-containing silica of silica solution is 30%) with surfactant by being surpassed Acoustic shock is swung, and increases the active group inside silica solution by surfactant, then it mix with butyl titanate etc. and is added Heat forms surface high-activity titanium silicon particle using the effect of template, then it is mixed with resorcinol, functive etc. Reaction forms surface grafting dissaving polymer ionic species, is then mixed, be prepared with adjuvant, mixture again Cashmere bleach-activating；

(2) present invention in use, first with the dissaving polymer ionic species in activator can effectively with Pigment is combined, and destroys pigment and the direct unsaturated bond of pigment, so that chromatophagous conjugated system, increases hydrogen peroxide Bleaching effect increase resolution ratio secondly by the decomposition of titanium silicon particle therein catalysis hydrogen peroxide, and pass through titanium silicon The effect of grain can the tert-butyl alcohol, cyclohexanone effectively in catalytic mixing material

It is that ammonium hydroxide is reacted with adjuvant, generates cyclohexanone oxime, the decomposability of hydrogen peroxide can be improved by reaction process Can, bleaching effect is improved, in addition cyclohexanone oxime can be reacted with hydrogen peroxide, generate better oxidation bleaching effect, be increased Strong bleachability.

Specific embodiment

Surfactant are as follows: sodium cocoyl methyl sodium taurocholate, lauroylamidopropyl betaine, Coconut Fatty Acid Monoethanolamide In any one.

Template is dodecyl sodium sulfate, cetyl trimethylammonium bromide 1:8~10 in mass ratio are stirred, i.e., Obtain template.

Functive is N- methylimidazole, bromo- 4- nitroimidazole 9:2~4 in mass ratio 2- mix.

Auxiliary agent is epoxychloropropane, acrylamide 6~9:2 in mass ratio is mixed.

Additive is urea, ammonium hydrogen carbonate, any one in sodium bicarbonate.

Mixed solvent is ethanol solution, 7:1~3 mix N,N-dimethylformamide by volume.

Mixture is the tert-butyl alcohol, cyclohexanone 9:1~6 in mass ratio mix.

Adjuvant is that sodium acetate is mixed with ammonium hydroxide 1:10~13 in mass ratio.

Stabilizer is sodium dihydrogen phosphate.

A kind of preparation method of cashmere bleach-activating, the preparation method include the following steps:

(1) it takes silica solution, surfactant and ethanol solution 7~9:1:20 in mass ratio to carry out ultrasonic vibration 15min, is put into anti- It answers in kettle, the template of silica solution quality 20~25%, the butyl titanate of silica solution quality 20~25% is added, 50~60 DEG C carry out preheating 30min；

(2) after preheating, nitrogen protection is added the ethanol amine of silica solution quality 50~55%, is warming up to 90~95 DEG C, stirs 3h is mixed, is cooled to 45~50 DEG C, stands 6h, is discharged, dried object is collected in spray drying；

(3) according to parts by weight, take 160~180 parts of mixed solvents, 40~50 parts of dried objects, 12~14 parts of resorcinols, 11~ 13 parts of trimellitic anhydrides, 10~13 parts of functives, 4~10 parts of auxiliary agents, 1~3 part of additive；

(4) mixed solvent, dried object, resorcinol, trimellitic anhydride and auxiliary agent are put into reaction kettle first, nitrogen protection, 125~130 DEG C are warming up to, 3~7h is stirred to react, is cooled to 105~110 DEG C, adds functive and additive, stirs 8h, It is cooled to room temperature, discharges, material out is mixed with ether 4:7~9 in mass ratio, stand, filtering collects filter residue, uses ether Washing, it is dry, collect dried object A；

(5) dried object A, mixture, adjuvant and stabilizer 7~9:3:1 in mass ratio~3:0.2 are uniformly mixed to get sheep Suede bleach-activating.