CN104313868B - Scouring and bleaching compositions and the application process of low temperature oxygen bleaching activator - Google Patents
Scouring and bleaching compositions and the application process of low temperature oxygen bleaching activator Download PDFInfo
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- CN104313868B CN104313868B CN201410563051.5A CN201410563051A CN104313868B CN 104313868 B CN104313868 B CN 104313868B CN 201410563051 A CN201410563051 A CN 201410563051A CN 104313868 B CN104313868 B CN 104313868B
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Abstract
The formula of scouringing and bleaching of a kind of low temperature oxygen bleaching activator of disclosure, comprises following material in every liter of water: scouring agent 1.0g, solid NaOH5.0g, hydrogen peroxide 4.5g, low temperature oxygen bleaching activator 3.0g; Low temperature oxygen bleaching activator includes synthetic intermediate and generates two stages of low temperature oxygen bleaching activator, wherein, the step of synthetic intermediate: 1) add diamine compounds, organic amine nertralizer, solvent orange 2 A, heat to solvent orange 2 A backflow; 2) solvent orange 2 A dissolves 4-dimethylamino Benzenecarbonyl chloride., insulation backflow; 3) precipitate out precipitate, obtain intermediate; Generate the step of low temperature oxygen bleaching activator: add intermediate, solvent B, drip dimethyl sulfate, stir 1-2 hour; Boil off solvent again, obtain low temperature oxygen bleaching activator; Described diamine compounds includes ethylene urea or carbamide, dicyandiamide. Fabric whiteness after scouringing and bleaching, capillary effect, brute force all can reach conventional level, and feel is better than common process.
Description
Technical field
The present invention relates to the pre-treatment field of the non-finished product textile of cellulose fibre, specifically, relate to scouring and bleaching formula and the using method of a kind of a kind of new type low temperature oxygen bleaching activator being applied in textile printing and dyeing pre-treatment.
Background technology
Printing and dyeing assistant industry face price rise steadily, charges for disposing pollutants rise and Export Textiles by technology barriers, domestic working ability more than the severe situation of demand, intensified competition, country also requires that " unit GDP energy resource consumption reduces by 20%, and total emissions of major pollutants reduces 10% " in Eleventh Five-Year Plan simultaneously. Therefore, printing and dyeing mill is concentrated mainly on reduction energy consumption sight, reduces processing cost, shortens the process-cycle and improve the aspects such as end product quality, to improve competitiveness. Printing and dyeing pre-treatment is the key procedure of a high energy consumption height blowdown, and along with the continuous rising of energy expenditure, the energy cost in pretreatment procedure seriously constrains the benefit of enterprise, so energy-conservation short-flow pre-treating process becomes the focus and emphasis of current research.
Conventional pre-treatment Scouring and bleaching process is all carry out in 100 DEG C even high-temperature high-pressure apparatus of 135 DEG C, and scouring and bleaching time 60-90min, consumes quantity of steam very big, and 1 ton of wollen fabrics about needs steam 5-6 ton, takies about the 60% of whole dyeing and finishing steam consumption, and power consumption is big; Additionally, traditional handicraft is because using a large amount of Caustic soda, it can generate sodium cellulosate with fibrin reaction, not easily washes from fiber, must repeatedly wash after scouringing and bleaching, and water consumption of scouringing and bleaching accounts for about the 50% of whole dyeing and finishing water consumption, and water consumption is big; Meanwhile, the discharge capacity of sewage and the expense of sewage disposal have also been accordingly increased.
At H2O2Bleaching bath adds the peroxide activated thing of people, is greatly improved H2O2The effect of bleaching under lower temperature and pH value condition, current oxygen bleaching activator mainly has tetraacetyl ethylene diamine (TAED), nonanoyloxybenzene sulfonate (NOBS), four acetyl glycosides urea (TAGU), five acetyl glucose (PAG) etc., the mechanism of action is for TAED, TAED and HOO-Nucleophilic substitution is occurred to generate peracetic acid anion, peracetic acid anion ratio H2O2Bleachability higher, strong discoloration can be produced when low temperature, low pH value, make fabric obtain good whiteness.But, in bleaching process, bleach is except destroying natural pigment, and cotton fiber itself can be influenced by damage. The damage of fiber occurs mainly in bleaching process, and the protective effect of fiber is substantially better than conventional pre-treatment by low temperature pre-treatment, and its main cause is that cold bleaching condition is gentleer, and fibre damage is less. Therefore, a kind of novel, gentle, easy low temperature oxygen bleaching activator is developed imperative.
Such that it is able to shorten the process time, improve production efficiency, save the consumption of steam and electricity, and treatment pressure of sewage can be alleviated, reduce waste water control expense.
Summary of the invention
The present invention is directed to current fabric pretreatment scouring and bleaching process length consuming time, steam demand amount is big, power consumption is big, treatment pressure of sewage weight problem, scouring and bleaching formula and the method for a kind of low temperature oxygen bleaching activator are provided, make the fabric whiteness after scouringing and bleaching, capillary effect, the powerful level that all can reach conventional Scouring and bleaching process, and feel is better than common process. This low temperature oxygen bleaching activator reacts formation peracetic acid compound in oxygen bleaching process with hydrogen peroxide, the temperature of hydrogen peroxide bleaching can be effectively reduced, bleaching-bathing can be practiced with scouring agent, hydrogen peroxide at low temperatures and process the non-finished product textile of cellulose fibre, to solve the deficiencies in the prior art.
It is a further object of the present invention to provide the using method of the formula of scouringing and bleaching of above-mentioned low temperature oxygen bleaching activator.
The technical solution used in the present invention: the formula of scouringing and bleaching of a kind of low temperature oxygen bleaching activator, comprises following material in every liter of water: scouring agent 1.0g, solid NaOH5.0g, hydrogen peroxide 4.5g, low temperature oxygen bleaching activator 3.0g; Described low temperature oxygen bleaching activator includes synthetic intermediate and generates two stages of low temperature oxygen bleaching activator, and wherein, the step of synthetic intermediate includes:
1) in four-hole boiling flask, add diamine compounds, organic amine nertralizer, solvent orange 2 A, heat to solvent orange 2 A backflow;
2) with solvent orange 2 A, 4-dimethylamino Benzenecarbonyl chloride. is dissolved, be then added in four-hole boiling flask, insulation backflow 5-6 hour;
3) cooling precipitates out precipitate, by precipitate sucking filtration, clean, drying, obtains intermediate;
The step generating low temperature oxygen bleaching activator includes:
4) in four-hole boiling flask, add intermediate, solvent B, and be slowly added dropwise dimethyl sulfate, time for adding 1-2 hour, continues stirring 1-2 hour after dripping off;
5) boil off solvent, obtain low temperature oxygen bleaching activator;
Described diamine compounds includes ethylene urea or carbamide, dicyandiamide.
Preferably, described organic amine nertralizer includes triethylamine or triethanolamine, pyridine. Organic amine neuutralizer is used for neutralizing the hydrogen chloride that course of reaction generates.
Preferably, described solvent orange 2 A includes toluene or dimethylbenzene, and described solvent B is acetonitrile.
The method of the formula of scouringing and bleaching of above-mentioned low temperature oxygen bleaching activator, comprises the following steps:
1) it is equipped with body lotion by bath raio 1:10, when heating to 30 DEG C, fabric is put into stirring in body lotion and runs 5min, then body lotion is warmed up to 60 DEG C with the speed of 2 DEG C/min;
2) insulation dipping bath 60min;
3) 60 DEG C of clear water washing 10min, wash with cold water after draining again;
4) dehydration, drying.
Compared with prior art, the invention have the advantages that
(1) saving the energy: temperature of routine being scouringed and bleaching 100 DEG C is down to 60 DEG C, low temperature process relatively traditional handicraft reduces energy consumption more than 50%, and energy-conserving action is notable.
(2) using water wisely: because the low temperature more traditional alkaline oxygen bath of Scouring and bleaching process amount of caustic soda is low, avoid the generation of a large amount of cellulose sodium salt, make washing be easier to, make original 1 ton of cotton scouring and bleaching and be reduced to 30-40 ton with water from 60 tons, saving half, quantity of wastewater effluent also reduces accordingly simultaneously;
(3) saving process time: because washing easily, heating up and temperature fall time reduces and washing times reduces, thus saving process time, generally can make to shorten to about 80% process time, dye-works's time efficiency is improved.
Detailed description of the invention
Below by way of detailed description of the invention, the invention will be further described.
The low temperature oxygen bleaching activator of the present invention, with 4-chloromethyl benzoic acid chlorides, aminated compounds for primary raw material, is prepared from by two-step reaction.
Above-mentioned low temperature oxygen bleaching activator is prepared by following steps:
One, synthetic intermediate: equipped with nitrogen protection, condensation reflux unit four-hole boiling flask in add diamine compounds, organic amine nertralizer, solvent orange 2 A; heat to solvent orange 2 A backflow; then with a small amount of solvent orange 2 A, 4-dimethylamino Benzenecarbonyl chloride. is dissolved; it is then added in four-hole boiling flask; insulation backflow 5-6 hour; reaction is slowly cooled to precipitation occur after terminating, sucking filtration is precipitated thing, and clean drying obtains intermediate. Diamine compounds includes ethylene urea, carbamide, dicyandiamide; Wherein organic amine nertralizer is mainly used to neutralize the hydrogen chloride generated in course of reaction, and it includes triethylamine, triethanolamine, pyridine; Solvent orange 2 A includes toluene, dimethylbenzene.
Two, synthesis low temperature oxygen bleaching activator: equipped with nitrogen protection, condensation reflux unit four-hole boiling flask in add intermediate, acetonitrile (solvent B); and it is slowly added dropwise dimethyl sulfate; time for adding is 1-2 hour; drip off follow-up continuation of insurance temperature 1-2 hour; then boiling off solvent, gained solid is low temperature oxygen bleaching activator.
Below, enumerate three embodiments illustrate it is a preparation process for the low temperature oxygen bleaching activator of invention:
Embodiment one: 1# low temperature oxygen bleaching activator
Equipped with nitrogen protection, condensation reflux unit four-hole boiling flask in add ethylene urea 4.3g, triethylamine 15g, toluene 110 milliliters; heat to refluxing toluene; it is subsequently adding the toluene 40 milliliters dissolved with 18.3g4-dimethylamino Benzenecarbonyl chloride.; insulation backflow 6 hours; it is slowly cooled to that precipitation occurs; sucking filtration is precipitated thing, and clean drying obtains 16.3g intermediate 1#, and productivity is 86%.
Equipped with nitrogen protection, condensation reflux unit four-hole boiling flask in add above-mentioned gained intermediate 11.37g, acetonitrile 120 milliliters; and it is slowly added dropwise dimethyl sulfate 6.3g; time for adding is 1 hour; stirring 2 hours is continued after dripping off; then boiling off solvent, gained solid is 1# low temperature oxygen bleaching activator.
Embodiment two: 2# low temperature oxygen bleaching activator
Equipped with nitrogen protection, condensation reflux unit four-hole boiling flask in add carbamide 3g, triethanolamine 22.4g, dimethylbenzene 110 milliliters; heat to refluxing xylene; it is subsequently adding the dimethylbenzene 40 milliliters dissolved with 18.3g4-dimethylamino Benzenecarbonyl chloride.; insulation backflow 6 hours; it is slowly cooled to that precipitation occurs; sucking filtration is precipitated thing, and clean drying obtains 13.8g intermediate 2#, and productivity is 78%.
Equipped with nitrogen protection, condensation reflux unit four-hole boiling flask in add intermediate 10.6g, acetonitrile 120 milliliters; and it being slowly added dropwise dimethyl sulfate 6.3g, time for adding is 90min, continues stirring 90min after dropping; then boiling off solvent, gained solid is 2# low temperature oxygen bleaching activator.
Embodiment three: 3# low temperature oxygen bleaching activator
Equipped with nitrogen protection, condensation reflux unit four-hole boiling flask in add dicyandiamide 4.2g, pyridine 11.8g, toluene 110 milliliters; heat to refluxing toluene; it is subsequently adding the toluene 40 milliliters dissolved with 18.3g4-dimethylamino Benzenecarbonyl chloride.; insulation backflow 5 hours; it is slowly cooled to that precipitation occurs; sucking filtration is precipitated thing, and clean drying obtains 14.3g intermediate 3#, and productivity is 76%.
Equipped with nitrogen protection, condensation reflux unit four-hole boiling flask in add intermediate 11.3g, acetonitrile 120 milliliters; and it being slowly added dropwise dimethyl sulfate 6.3g, time for adding is 2 hours, continues stirring 1 hour after dripping off; then boiling off solvent, gained solid is 3# low temperature oxygen bleaching activator.
Use above-mentioned three kinds of low temperature oxygen bleaching activators, practice bleaching-bathing with scouring agent, hydrogen peroxide, NaOH respectively and process the non-finished product textile of cellulose fibre, and compare with common process, the bleaching effect of formula of scouringing and bleaching from test data detection low temperature oxygen bleaching activator of the present invention.
The low temperature using 1#, 2#, 3# oxygen bleaching activator is scouringed and bleaching formula
Oxygen bleaching activator (1#, 2#, 3#) 3.0g/L
Scouring agent DM-13611.0g/L
Solid NaOH5.0g/L
100%H2O24.5g/L
Above-mentioned formula is equipped with body lotion by bath raio 1:10, fabric is put in body lotion when heating to 30 DEG C and first run 5min, then body lotion is warmed up to 60 DEG C with the speed of 2 DEG C/min, after insulation 60min, body lotion is discharged, then 60 DEG C of clear water washing 10min, washing 5min, dewatered drying with cold water again after draining, get damp again 2h. Test fabric whiteness, capillary effect, brute force, feel, detection data are in Table 1.
Existing routine formula of scouringing and bleaching is:
Tradition refining agent 0.5g/L
Solid NaOH2.0g/L
100%H2O21.5g/L
Hydrogen peroxide stabilizer 1.0g/L
Above-mentioned formula is equipped with body lotion by bath raio 1:10, fabric is put in body lotion when heating to 30 DEG C and first run 5min, then body lotion is warmed up to 98 DEG C with the speed of 2 DEG C/min, cool to 80 DEG C after insulation 45min, body lotion is discharged, then 90 DEG C of clear water washing 10min, 5min is washed with cold water again after draining, dewatered drying, get damp again 2h, test fabric whiteness, capillary effect, brute force, feel. Detection data are in Table 1.
Table 1 Scouring and bleaching process performance comparison
The present invention uses low temperature oxygen bleaching activator, build hydrogen peroxide, system scouringed and bleaching by activator, adopt water-bath processing method, reach the good bleaching effect to fabric, the whiteness making fabric keeps the level with conventional bleaching and feel to be better than conventional bleaching, thus the damage of fabric can be reduced, and reduces energy consumption, improve production efficiency, for the ecological, environmental protective, energy-saving and cost-reducing significant of dyeing industry.
Claims (4)
1. the compositions of scouringing and bleaching of a low temperature oxygen bleaching activator, it is characterised in that comprise following material in every liter of water: scouring agent 1.0g, solid NaOH5.0g, hydrogen peroxide 4.5g, low temperature oxygen bleaching activator 3.0g; The preparation method of low temperature oxygen bleaching activator includes synthetic intermediate and generates two stages of low temperature oxygen bleaching activator, and wherein, the step of synthetic intermediate includes:
1) in four-hole boiling flask, add diamine compounds, organic amine nertralizer, solvent orange 2 A, heat to solvent orange 2 A backflow;
2) with solvent orange 2 A, 4-dimethylamino Benzenecarbonyl chloride. is dissolved, be then added in four-hole boiling flask, insulation backflow 5-6 hour;
3) cooling precipitates out precipitate, by precipitate sucking filtration, clean, drying, obtains intermediate;
The step generating low temperature oxygen bleaching activator includes:
4) in four-hole boiling flask, add intermediate, solvent B, and be slowly added dropwise dimethyl sulfate, time for adding 1-2 hour, continues stirring 1-2 hour after dripping off;
5) boil off solvent, obtain low temperature oxygen bleaching activator;
Described diamine compounds includes ethylene urea or carbamide or dicyandiamide.
2. the compositions of scouringing and bleaching of low temperature oxygen bleaching activator according to claim 1, it is characterised in that: described organic amine nertralizer includes triethylamine or triethanolamine or pyridine, and organic amine neuutralizer is used for neutralizing the hydrogen chloride that course of reaction generates.
3. the compositions of scouringing and bleaching of low temperature oxygen bleaching activator according to claim 1, it is characterised in that: described solvent orange 2 A includes toluene or dimethylbenzene, and described solvent B is acetonitrile.
4. the application process of the compositions of scouringing and bleaching of low temperature oxygen bleaching activator described in a claim 1, it is characterised in that comprise the following steps:
1) it is equipped with body lotion by bath raio 1:10, when heating to 30 DEG C, fabric is put into stirring in body lotion and runs 5min, then body lotion is warmed up to 60 DEG C with the speed of 2 DEG C/min;
2) insulation dipping bath 60min;
3) 60 DEG C of clear water washing 10min, wash with cold water after draining again;
4) dehydration, drying.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3775333A (en) * | 1972-06-30 | 1973-11-27 | American Cyanamid Co | N-acyl azolinones as peroxygen bleach activators |
| US4115059A (en) * | 1977-10-03 | 1978-09-19 | Fmc Corporation | Aromatic sulfonyl fluorides as peroxygen activators |
| US4167487A (en) * | 1973-06-07 | 1979-09-11 | Colgate-Palmolive Company | Aromatic activator |
| CN1124038A (en) * | 1993-05-20 | 1996-06-05 | 普罗格特-甘布尔公司 | Bleaching compositions comprising peroxyacid activators having amide moieties |
| US5998350A (en) * | 1993-05-20 | 1999-12-07 | The Procter & Gamble Company | Bleaching compounds comprising N-acyl caprolactam and/or peroxy acid activators |
| CN101037842A (en) * | 2007-04-19 | 2007-09-19 | 上海祺瑞纺织化工有限公司 | Low-temperature scouring and bleaching agent and preparation method thereof and preprocessing technique |
-
2012
- 2012-03-15 CN CN201410563051.5A patent/CN104313868B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3775333A (en) * | 1972-06-30 | 1973-11-27 | American Cyanamid Co | N-acyl azolinones as peroxygen bleach activators |
| US4167487A (en) * | 1973-06-07 | 1979-09-11 | Colgate-Palmolive Company | Aromatic activator |
| US4115059A (en) * | 1977-10-03 | 1978-09-19 | Fmc Corporation | Aromatic sulfonyl fluorides as peroxygen activators |
| CN1124038A (en) * | 1993-05-20 | 1996-06-05 | 普罗格特-甘布尔公司 | Bleaching compositions comprising peroxyacid activators having amide moieties |
| US5998350A (en) * | 1993-05-20 | 1999-12-07 | The Procter & Gamble Company | Bleaching compounds comprising N-acyl caprolactam and/or peroxy acid activators |
| CN101037842A (en) * | 2007-04-19 | 2007-09-19 | 上海祺瑞纺织化工有限公司 | Low-temperature scouring and bleaching agent and preparation method thereof and preprocessing technique |
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Address after: 528300 Guangdong, Shunde District, Guangzhou Zhuhai Road, the sea side of the road Patentee after: Guangdong Demei fine chemical group Limited by Share Ltd Address before: 528300 Guangdong, Shunde District, Guangzhou Zhuhai Road, the sea side of the road Patentee before: Guangdong Demei Fine Chemical Co., Ltd. |