CN102605651A - Preparation method of novel leveling agent - Google Patents
Preparation method of novel leveling agent Download PDFInfo
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- CN102605651A CN102605651A CN2012100766242A CN201210076624A CN102605651A CN 102605651 A CN102605651 A CN 102605651A CN 2012100766242 A CN2012100766242 A CN 2012100766242A CN 201210076624 A CN201210076624 A CN 201210076624A CN 102605651 A CN102605651 A CN 102605651A
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Abstract
The invention belongs to the field of production of the textile printing and dyeing industry, and particularly relates to a preparation method of a leveling agent. The preparation method of the novel leveling agent is characterized by comprising the following steps of: (1) synthesizing hydroxymethyl alkylphenol polyoxyethylene ether: taking alkylphenol polyoxyethylene ether, adding formaldehyde, adding potassium hydrate or sodium hydrate, distilling and reacting at the reacting temperature of 80-125 DEG C till no distillate appears to obtain hydroxymethyl alkylphenol polyoxyethylene ether, wherein the molar ratio of alkylphenol polyoxyethylene ether to formaldehyde is 1:(0.2-2), and the mixture ratio of the alkylphenol polyoxyethylene ether to the potassium hydrate or sodium hydrate is 323.0g:4.0g; and (2) uniformly mixing the hydroxymethyl alkylphenol polyoxyethylene ether with a higher fatty acid salt in boiling water bath in the mass ratio of 1:(0.1-16) to obtain the leveling agent. The leveling agent prepared by the method has a good leveling effect.
Description
Technical field
The invention belongs to the textile printing and dyeing industry production field, be specifically related to a kind of preparation method of levelling agent.
Background technology
Dyed fiber under hot conditions, the mean kinetic energy of its macromolecular chain improves rapidly.Along with the rising of temperature, the athletic meeting of being dyed the fiber macromolecular chain forms numerous spaces in fiber, and the molecule of DISPERSE DYES is spread in fiber by thermal excitation also simultaneously, and in fiber, accumulates abundant dye molecule, thereby accomplishes the process of dying.Owing to dyed the interactional complexity of various auxiliary agent dyestuffs in the dispersion unstability, dye bath of otherness, the DISPERSE DYES of fiber itself structure and physical state of living in; The fluctuation that also has dyeing course intensification and constant temperature; Overcome these unfavorable factors to reach even dyeing effect, just must use levelling agent.
The levelling agent that in high-temperature dyeing process, uses roughly has three kinds:
The one, contain the levelling agent of ethyoxyl structure.Its function is in dyeing course, to capture DISPERSE DYES, increases the seat of dyeing, delays to dye to have reached even dyeing effect.But it is prone to cause dyestuff to associate and coacervation occurs.
The 2nd, contain the levelling agent of aromatic compound.Its essence is a kind of carrier.Its function is when the dyeing intensification reaches a certain critical value; Make and dye fiber and produce the speedup swelling rapidly; And intrastitial space is significantly increased; Impel also rapid and concentrated the dying in fiber of dyestuff, it causes the continuous desorb of intrastitial dyestuff to break away from fiber and tangible migration takes place as the solvent of dyestuff again simultaneously.This had both helped improving the dyeing inequality that rapid dyeing causes, but had also obviously reduced the dye-uptake of dyestuff.
The 3rd, contain the levelling agent of aliphatic compound, it has the advantage of above-mentioned two kinds of levelling agents concurrently, can under the condition of different temperatures of dyeing, have both short dying and gentlely dye function, increases the migration of DISPERSE DYES greatly, thereby makes high-temp dyeing reach effect of uniform.But because its relative molecular weight is bigger, level dyeing efficient is lower, required levelling agent large usage quantity.
Because all there is certain limitation in above-mentioned levelling agent, so need it is optimized.
Summary of the invention
Problem to be solved by this invention is the limitation to above-mentioned conventional high-temperature levelling agent, and a kind of preparation method of novel levelling agent is provided, and the levelling agent of this method preparation has good even dyeing effect.
The technical scheme that the present invention taked is: a kind of preparation method of novel levelling agent is characterized in that it comprises the steps:
1) the hydroxymethyl alkyl phenol polyethenoxy ether is synthetic: the mol ratio by APES and formaldehyde is 1: 0.2～2; Proportioning by APES and potassium hydroxide or NaOH is 323.0g: 4.0g; Get APES, add formaldehyde, add potassium hydroxide or NaOH (making catalyst) with potassium hydroxide or NaOH; In reaction temperature is to distill, react under 80 ℃～125 ℃ (to adopt the indirect mode; Distill, react having under the condition of backflow), occur to there being distillate, obtain the hydroxymethyl alkyl phenol polyethenoxy ether;
2) mass ratio by hydroxymethyl alkyl phenol polyethenoxy ether and higher fatty acid salt is 1: 0.1～16, with hydroxymethyl alkyl phenol polyethenoxy ether (A) and higher fatty acid salt boiling water bath mixing, obtains levelling agent.
Press such scheme, APES is a kind of in NPE-8, NPE-10, the NPE-12.
Press such scheme, the mol ratio of APES and formaldehyde is 1: 1～2.
Press such scheme, the mass ratio of hydroxymethyl alkyl phenol polyethenoxy ether and higher fatty acid salt is 2～5: 5～8.
Press such scheme, higher fatty acid salt can be a cottonseed oil fatty acid salt, also can be animal, plant fatty acid salt such as rapeseed oil fatty acid salt, tallow fatty acid sodium salt.Higher fatty acid salt can be the alkali metal sodium salt, also can be alkali metal sylvite, can also be alkali metal salts such as lithium salts.
Press such scheme, said higher fatty acid salt is produced from cotton oil distillation residues:
1) get 200g cotton oil distillation residues, 400g distilled water, 100mL dilute sodium hydroxide aqueous solution, wherein, the concentration of dilute sodium hydroxide aqueous solution is 10wt%～20wt%; In cotton oil distillation residues, add distilled water, and dilute sodium hydroxide aqueous solution, be heated to little boiling (temperature is 85 ℃～108 ℃) state, to leave standstill and be cooled to room temperature, the upper strata separator is got in layering, with vacuum filtration machine suction filtration under vacuum 0.01MPa～0.04MPa,
2) add the 50mL concentrated sodium hydroxide aqueous solution again; The concentration of the concentrated sodium hydroxide aqueous solution is 20wt%～30wt%, is heated to little boiling (temperature is 85 ℃～108 ℃, and alkali is analysed for the first time); Leave standstill and be cooled to room temperature; The upper strata separator is got in layering, uses vacuum filtration machine suction filtration under vacuum 0.01MPa～0.04MPa again;
3) repeating step 2) 2～5 times, the upper strata separator behind the suction filtration is added in the 100mL distilled water, be heated to little boiling (temperature is 85 ℃～108 ℃); Leave standstill and be cooled to room temperature; The upper strata separator is got in layering, uses vacuum filtration machine suction filtration under vacuum 0.01Mpa～0.04MPa again; Upper strata separator behind low temperature (temperature is 55 ℃～68 ℃) the oven dry gained suction filtration, the higher fatty acids sodium that obtains.
Use: with the levelling agent that the makes experiment of dyeing: the proportioning by levelling agent, glacial acetic acid, NaOH, distilled water, dyestuff is 0.2g: 0.2mL: 0.1g: 600mL: 0.2g; Levelling agent, glacial acetic acid, NaOH are joined (the used container of dyeing experiment is a 1L thin-walled iron basin) in the distilled water; Stir; Water-bath to 50 ℃; Add dyestuff (used dyestuff is a disperse red FB/3B dyestuff), add behind the mixing and dye line (used one cotton fiber that dyes line for long 8cm), stir and 90 ℃ of water-bath 1h (mixing speed 3r/s); The line that dyes after the dyeing is dried (cotton thread after the dyeing is dried after need washing again) down at 55 ℃, the counterstain result confirms best proportioning.
Contrast through the dyeing experimental result; Confirm best proportioning; The mass ratio of hydroxymethyl alkyl phenol polyethenoxy ether and higher fatty acid salt is 4: 6, and the mol ratio of the NPE-10 during synthetic hydroxymethyl alkyl phenol polyethenoxy ether (A) and formaldehyde is 1: 1.4.
The invention has the beneficial effects as follows: the levelling agent of this method preparation has good even dyeing effect.
The present invention is applicable to 80 ℃～100 ℃ high-temperature dyeing industry.This levelling agent has combined the advantage of conventional high-temperature levelling agent (aromatic series polyoxyethylene compound and sodium soap).
The specific embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to following embodiment.
Embodiment 1:
A kind of preparation method of novel levelling agent, it comprises the steps:
1) the hydroxymethyl alkyl phenol polyethenoxy ether is synthetic:
Accurately taking by weighing " NPE " 323.0 gram, is 1: 1 by the mol ratio of NPE and formaldehyde, 1: 1.2; 1: 1.4,1: 1.6,1: 1.8; 1: 2, make catalyst with 4.0 gram potassium hydroxide, adopt distillation, reaction down for 105 ℃ in reaction temperature; The standard that reaction is accomplished is that tail is taken over no distillate appearance, obtains hydroxymethyl alkyl phenol polyethenoxy ether (A).
2) from cotton oil distillation residues, produce higher fatty acid salt:
1. get 200g cotton oil distillation residues (should be cotton oil distillation residues here), 400g distilled water, 100mL dilute sodium hydroxide aqueous solution, wherein, the concentration of dilute sodium hydroxide aqueous solution is 15wt%; In cotton oil distillation residues, add distilled water, and dilute sodium hydroxide aqueous solution, be heated to little boiling (temperature is 85 ℃～108 ℃) state; Leave standstill and be cooled to room temperature, (can see its obvious layering, the upper strata is faint yellow semifluid in layering; Lower floor is a black liquor), get upper strata separator (, isolating the upper strata semifluid) through filtering operation; With vacuum filtration machine suction filtration under vacuum 0.01Mpa～0.04MPa
2. add the 50mL concentrated sodium hydroxide aqueous solution again; The concentration of the concentrated sodium hydroxide aqueous solution is 25wt%, is heated to little boiling (temperature is 85 ℃～108 ℃, and alkali is analysed for the first time); Leave standstill and be cooled to room temperature; The upper strata separator is got in layering, uses vacuum filtration machine suction filtration under vacuum 0.01Mpa～0.04MPa again;
3. 2. secondary (three alkali are analysed altogether) of repeating step after three alkali are analysed, adds the upper strata separator behind the suction filtration in the 100mL distilled water; Be heated to little boiling (temperature is 85 ℃～108 ℃), leave standstill and be cooled to room temperature, layering; Get the upper strata separator, use vacuum filtration machine suction filtration under vacuum 0.01Mpa～0.04MPa again, the upper strata separator behind low temperature (temperature is 55 ℃～68 ℃) the oven dry gained suction filtration; The higher fatty acids sodium (B) that obtains is faint yellow soap shape thing.
3) mass ratio by hydroxymethyl alkyl phenol polyethenoxy ether and higher fatty acids sodium (B) is 5: 5,4.5: 5.5, and 4: 6; 3.5: 6.5,3: 7,2.5: 7.5; 2: 8,, obtain 42 groups of levelling agents with hydroxymethyl alkyl phenol polyethenoxy ether (A) and higher fatty acids sodium (B) boiling water bath mixing.
Application example 1
This experiment is according to A: the B proportioning is the experiment of dyeing in 5: 5, take by weighing the 0.2g levelling agent (A wherein: the mol ratio of NPE and formaldehyde has 1: 1,1: 1.2,1: 1.4; 1: 1.6,1: 1.8,1: 2); 0.1g NaOH pipettes 0.2mL acetic acid (glacial acetic acid) with the 0.50mL pipette, adds 600.0mL distilled water; Stir with 3r/s, water-bath is heated to 50 ℃, adds 0.2g disperse red FB/3B dyestuff; Stir after one minute, add one cotton thread (cotton fiber) of long 8cm, 90 ℃ of water-bath 1h.Then cotton thread is taken out,, put into 55 ℃ of baking ovens again and dry with running water flush away residual dye liquor wherein.Obtain six groups and dye line, the dyeing flower phenomenon is arranged, chroma is medium, and the levelling agent that the preparation of this method is described has good even dyeing effect (below identical).
Application example 2
This experiment is according to A: the B proportioning is the experiment of dyeing in 4.5: 5.5, take by weighing the 0.2g levelling agent (A wherein: the proportioning of NPE and formaldehyde has 1: 1,1: 1.2,1: 1.4; 1: 1.6,1: 1.8,1: 2), 0.1g NaOH; Pipette 0.2mL acetic acid with the 0.50mL pipette, add 600.0mL distilled water, stir with 3r/s, water-bath is heated to 50 ℃; Add 0.2g disperse red FB/3B dyestuff, stir after one minute, add one cotton thread of long 8cm, 90 ℃ of water-bath 1h.Then cotton thread is taken out,, put into 55 ℃ of baking ovens again and dry with running water flush away residual dye liquor wherein.Obtain six groups and dye line, except that A: B=1: all occur slight dyeing flower 1.4, chroma is slightly high.
Application example 3
This experiment is according to A: the B proportioning is the experiment of dyeing in 4: 6, take by weighing the 0.2g levelling agent (A wherein: the mol ratio of NPE and formaldehyde has 1: 1,1: 1.2,1: 1.4; 1: 1.6,1: 1.8,1: 2), 0.1g NaOH; Pipette 0.2mL acetic acid with the 0.50mL pipette, add 600.0mL distilled water, stir with 3r/s, water-bath is heated to 50 ℃; Add 0.2g disperse red FB/3B dyestuff, stir after one minute, add one cotton thread of long 8cm, 90 ℃ of water-bath 1h.Then cotton thread is taken out,, put into 55 ℃ of baking ovens again and dry with running water flush away residual dye liquor wherein.Obtain six groups and dye line, all do not have the dyeing flower phenomenon, chroma is high.
Application example 4
This experiment is according to A: the B proportioning is the experiment of dyeing in 3.5: 6.5, take by weighing the 0.2g levelling agent (A wherein: the mol ratio of NPE and formaldehyde has 1: 1,1: 1.2,1: 1.4; 1: 1.6,1: 1.8,1: 2), 0.1g NaOH; Pipette 0.2mL acetic acid with the 0.50mL pipette, add 600.0mL distilled water, stir with 3r/s, water-bath is heated to 50 ℃; Add 0.2g disperse red FB/3B dyestuff, stir after one minute, add one cotton thread of long 8cm, 90 ℃ of water-bath 1h.Then cotton thread is taken out,, put into 55 ℃ of baking ovens again and dry with running water flush away residual dye liquor wherein.Obtain six groups and dye line, all do not have the dyeing flower phenomenon, chroma is slightly high.
Application example 5
This experiment is according to A: the B proportioning is the experiment of dyeing in 3: 7, take by weighing the 0.2g levelling agent (A wherein: the mol ratio of NPE and formaldehyde has 1: 1,1: 1.2,1: 1.4; 1: 1.6,1: 1.8,1: 2), 0.1g NaOH; Pipette 0.2mL acetic acid with the 0.50mL pipette, add 600.0mL distilled water, stir with 3r/s, water-bath is heated to 50 ℃; Add 0.2g disperse red FB/3B dyestuff, stir after one minute, add one cotton thread of long 8cm, 90 ℃ of water-bath 1h.Then cotton thread is taken out,, put into 55 ℃ of baking ovens again and dry with running water flush away residual dye liquor wherein.Obtain six groups and dye line, except that A: B=1: 1.4 and 1: 1.6 slight dyeing flower phenomenon is all arranged, chroma is medium.
Application example 6
This experiment is according to A: the B proportioning is the experiment of dyeing in 2.2: 7.5, take by weighing the 0.2g levelling agent (A wherein: the mol ratio of NPE and formaldehyde has 1: 1,1: 1.2,1: 1.4; 1: 1.6,1: 1.8,1: 2), 0.1g NaOH; Pipette 0.2mL acetic acid with the 0.50mL pipette, add 600.0mL distilled water, stir with 3r/s, water-bath is heated to 50 ℃; Add 0.2g disperse red FB/3B dyestuff, stir after one minute, add one cotton thread of long 8cm, 90 ℃ of water-bath 1h.Then cotton thread is taken out,, put into 55 ℃ of baking ovens again and dry with running water flush away residual dye liquor wherein.Obtain six groups and dye line, except that A: B=1: slight dyeing flower phenomenon is all arranged 1.4, and chroma is medium.
Application example 7
This experiment is according to A: the B proportioning is the experiment of dyeing in 2: 8, take by weighing the 0.2g levelling agent (A wherein: the mol ratio of NPE and formaldehyde has 1: 1,1: 1.2,1: 1.4; 1: 1.6,1: 1.8,1: 2), 0.1g NaOH; Pipette 0.2mL acetic acid with the 0.50mL pipette, add 600.0mL distilled water, stir with 3r/s, water-bath is heated to 50 ℃; Add 0.2g disperse red FB/3B dyestuff, stir after one minute, add one cotton thread of long 8cm, 90 ℃ of water-bath 1h.Then cotton thread is taken out,, put into 55 ℃ of baking ovens again and dry with running water flush away residual dye liquor wherein.Obtain six groups and dye line, the dyeing flower phenomenon is all arranged, chroma is on the low side.
The evaluation criterion of even dyeing effect is the level-dyeing property quality and chroma height of dying line, will dye line and contrast, and analyzes degree and color gorgeous puckery of its dyeing flower phenomenon, and wherein color is the most gorgeous, and the used proportioning of line of dying of no dyeing flower phenomenon is best proportioning.
Each raw material that the present invention is cited, and the bound of each raw material of the present invention, interval value, and the bound of technological parameter (like temperature, time etc.), interval value can both realize the present invention, do not enumerate embodiment one by one at this.
Claims (8)
1. the preparation method of a novel levelling agent is characterized in that it comprises the steps:
1) the hydroxymethyl alkyl phenol polyethenoxy ether is synthetic: the mol ratio by APES and formaldehyde is 1: 0.2～2; Proportioning by APES and potassium hydroxide or NaOH is 323.0g: 4.0g, gets APES, adds formaldehyde; Add potassium hydroxide or NaOH; In reaction temperature is to distill, react under 80 ℃～125 ℃, does not occur to there being distillate, obtains the hydroxymethyl alkyl phenol polyethenoxy ether;
2) mass ratio by hydroxymethyl alkyl phenol polyethenoxy ether and higher fatty acid salt is 1: 0.1～16, with hydroxymethyl alkyl phenol polyethenoxy ether and higher fatty acid salt boiling water bath mixing, obtains levelling agent.
2. the preparation method of a kind of novel levelling agent according to claim 1 is characterized in that: APES is a kind of in NPE-8, NPE-10, the NPE-12.
3. the preparation method of a kind of novel levelling agent according to claim 1, it is characterized in that: the mol ratio of APES and formaldehyde is 1: 1～2.
4. the preparation method of a kind of novel levelling agent according to claim 1, it is characterized in that: the mass ratio of hydroxymethyl alkyl phenol polyethenoxy ether and higher fatty acid salt is 2～5: 5～8.
5. the preparation method of a kind of novel levelling agent according to claim 1, it is characterized in that: higher fatty acid salt is cottonseed oil fatty acid salt, rapeseed oil fatty acid salt or tallow fatty acid sodium salt, or alkali metal sodium salt, alkali metal sylvite or lithium salts.
6. the preparation method of a kind of novel levelling agent according to claim 1, it is characterized in that: said higher fatty acid salt is produced from cotton oil distillation residues:
1) get 200g cotton oil distillation residues, 400g distilled water, 100mL dilute sodium hydroxide aqueous solution, wherein, the concentration of dilute sodium hydroxide aqueous solution is 10wt%～20wt%; In cotton oil distillation residues, add industrial running water, and dilute sodium hydroxide aqueous solution, be heated to slight boiling condition, to leave standstill and be cooled to room temperature, the upper strata separator is got in layering, with vacuum filtration machine suction filtration under vacuum 0.01MPa～0.04MPa,
2) add the 50mL concentrated sodium hydroxide aqueous solution again, the concentration of the concentrated sodium hydroxide aqueous solution is 20wt%～30wt%, is heated to little boiling, and leaves standstill and is cooled to room temperature, and the upper strata separator is got in layering, uses vacuum filtration machine suction filtration under vacuum 0.01MPa～0.04MPa again;
3) repeating step 2) 2～5 times, the upper strata separator behind the suction filtration is added in the 100mL distilled water, be heated to little boiling; Leave standstill and be cooled to room temperature; The upper strata separator is got in layering, uses vacuum filtration machine suction filtration under vacuum 0.01MPa～0.04MPa again; Upper strata separator behind the low temperature drying gained suction filtration, the higher fatty acids sodium that obtains.
7. the preparation method of a kind of novel levelling agent according to claim 6, it is characterized in that: little boiling is meant that temperature is 85 ℃～108 ℃.
8. the preparation method of a kind of novel levelling agent according to claim 6, it is characterized in that: low temperature is meant that temperature is 55 ℃～68 ℃.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103669043A (en) * | 2013-11-22 | 2014-03-26 | 南通市通州区川姜镇盛世王朝家用纺织品设计工作室 | Leveling agent for wool and real silk and preparation method thereof |
| CN103757945A (en) * | 2013-12-14 | 2014-04-30 | 常熟市淼泉盛达助剂厂 | Leveling agent for fabric |
| CN103790043A (en) * | 2013-11-29 | 2014-05-14 | 杭州美高华颐化工有限公司 | Environment-friendly high-temperature leveling agent and preparation method thereof |
| CN104278566A (en) * | 2013-07-02 | 2015-01-14 | 江苏省海安石油化工厂 | Preparation method for terylene dispersing and leveling agent |
| CN107044057A (en) * | 2016-12-30 | 2017-08-15 | 丁玉琴 | A kind of high-temperature stable is combined the preparation method of levelling agent |
| CN109294547A (en) * | 2018-10-23 | 2019-02-01 | 天津大港油田滨港集团博弘石油化工有限公司 | A kind of displacement of reservoir oil anionic and nonionic amphoteric surfactant and preparation method thereof |
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| CN1393596A (en) * | 2001-07-03 | 2003-01-29 | 张义忠 | Low-temp dyeing accelerant of dye |
| CN101328687A (en) * | 2008-07-25 | 2008-12-24 | 浙江理工大学 | Environment-friendly type terylene low temperature dyeing assistant with alkyl phthalic imide as vector and preparation thereof |
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| US4270917A (en) * | 1978-10-16 | 1981-06-02 | Imperial Chemical Industries Limited | Stabilized aqueous dyestuff dispersions |
| CN1393596A (en) * | 2001-07-03 | 2003-01-29 | 张义忠 | Low-temp dyeing accelerant of dye |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104278566A (en) * | 2013-07-02 | 2015-01-14 | 江苏省海安石油化工厂 | Preparation method for terylene dispersing and leveling agent |
| CN103669043A (en) * | 2013-11-22 | 2014-03-26 | 南通市通州区川姜镇盛世王朝家用纺织品设计工作室 | Leveling agent for wool and real silk and preparation method thereof |
| CN103669043B (en) * | 2013-11-22 | 2015-10-28 | 南通市通州区川姜镇盛世王朝家用纺织品设计工作室 | Wool real silk levelling agent and preparation method thereof |
| CN103790043A (en) * | 2013-11-29 | 2014-05-14 | 杭州美高华颐化工有限公司 | Environment-friendly high-temperature leveling agent and preparation method thereof |
| CN103757945A (en) * | 2013-12-14 | 2014-04-30 | 常熟市淼泉盛达助剂厂 | Leveling agent for fabric |
| CN107044057A (en) * | 2016-12-30 | 2017-08-15 | 丁玉琴 | A kind of high-temperature stable is combined the preparation method of levelling agent |
| CN109294547A (en) * | 2018-10-23 | 2019-02-01 | 天津大港油田滨港集团博弘石油化工有限公司 | A kind of displacement of reservoir oil anionic and nonionic amphoteric surfactant and preparation method thereof |
| CN109294547B (en) * | 2018-10-23 | 2020-11-20 | 天津大港油田滨港集团博弘石油化工有限公司 | Anionic and nonionic amphoteric surfactant for oil displacement and preparation method thereof |
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