CN104141251B - A kind of synthesis preparation method of Superfine Fibre Fabric high temperature levelling agent - Google Patents
A kind of synthesis preparation method of Superfine Fibre Fabric high temperature levelling agent Download PDFInfo
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- CN104141251B CN104141251B CN201410125362.3A CN201410125362A CN104141251B CN 104141251 B CN104141251 B CN 104141251B CN 201410125362 A CN201410125362 A CN 201410125362A CN 104141251 B CN104141251 B CN 104141251B
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Abstract
The present invention relates to a kind of high temperature levelling agent, relate in particular to a kind of synthesis preparation method of Superfine Fibre Fabric high temperature levelling agent, belong to textile auxiliary's technical field. Carry out according to the following steps: high temperature levelling agent A component synthetic → high temperature levelling agent B component synthetic → high temperature levelling agent C component synthetic → composite. The better permeance property of synthesis preparation method of Superfine Fibre Fabric high temperature levelling agent, therefore can make dyestuff be penetrated into comparatively easily superfine fibre inside under the effect of levelling agent to play the effect of level dyeing.
Description
Technical field
The present invention relates to a kind of high temperature levelling agent, relate in particular to a kind of synthetic preparation of Superfine Fibre Fabric high temperature levelling agentMethod, belongs to textile auxiliary's technical field.
Background technology
Superfine Fibre Fabric has advantages of high-hydroscopicity, strong dirt-removing, does not lose hair or feathers, life-span length, easy cleaning, do not fade,People are constantly promoted for the demand of superfine fibre, but the characteristic of superfine fibre high-count and high-density make the even of dyeingUniformity difficulty is larger than general fiber, and first dyestuff must be penetrated into superfine fibre inside well, traditional high temperature level dyeingAgent, because molecular weight is large, carbon chain length is unfavorable for helping dyestuff penetration to fibrous inside, finally causes Dyeing of Superfine Polyester Fibre processIn often occur dyeing non-uniform phenomenon.
Summary of the invention
The present invention solves the deficiencies in the prior art, solves better inhomogeneous the asking of Dyeing of Superfine Polyester FibreTopic, the synthesis preparation method of a kind of Superfine Fibre Fabric high temperature levelling agent of raising Dyeing of Superfine Polyester Fibre one-time success rate.
Above-mentioned technical problem of the present invention is mainly solved by following technical proposals:
A synthesis preparation method for Superfine Fibre Fabric high temperature levelling agent, carries out according to the following steps:
(1), high temperature levelling agent A component is synthetic:
Taking aliphatic acid and polyethylene glycol as raw material, under strong acid catalyst effect, carry out esterification, the synthetic high temperature that obtainsLevelling agent A component;
Aliphatic acid is 1～2:1 with the ratio of the amount of substance of polyethylene glycol;
The amount of strong acid catalyst is 0.5%～1% of aliphatic acid and polyethylene glycol quality summation;
(2), high temperature levelling agent B component is synthetic:
Phenol APEO, urea and sulfamic acid are carried out to sulfonating reaction, obtain high temperature levelling agent B component;
The ratio of the amount of substance of phenol APEO, urea and sulfamic acid is 1:0.25～0.5:0.5～1;
(3), high temperature levelling agent C component is synthetic:
Adipic acid and poly glycol monomethyl ether are carried out to esterification under strong acid catalyst effect, and synthetic to obtain high temperature evenStain C component;
The ratio of the amount of substance of adipic acid and poly glycol monomethyl ether is 1:2;
The amount of strong acid catalyst is 0.5～1% of adipic acid and poly glycol monomethyl ether quality summation;
(4), composite: by the preparing burden by weight of the high temperature levelling agent in above each step:
20～62 parts of high temperature levelling agent A components
6～18 parts of high temperature levelling agent B components
4～20 parts of high temperature levelling agent C components
5～10 parts of isopropyl alcohols
15～65 parts, water
High temperature levelling agent A component, high temperature levelling agent B component, high temperature levelling agent C component are added in reactor successively, riseTemperature is to 60～70 degree, and the time of stirring is 30 minutes, adds water and opens cooling water and lower the temperature, when temperature is down to 30～40 degreeTime, close cooling water, then add isopropyl alcohol, then stir discharging 15 minutes.
As preferably, described aliphatic acid is any one in isooctyl acid, different n-nonanoic acid and isodecyl acid.
As preferably, the molecular size range of described polyethylene glycol is 400～800.
As preferably, described strong acid catalyst is more than 98% concentrated sulfuric acid, the p-methyl benzenesulfonic acid and 12 of mass fractionAny one in alkyl benzene sulphonate.
As preferably, the EO number of described phenol APEO is 3～7.
As preferably, in described poly glycol monomethyl ether structure, molecular weight polyethylene glycol is 200～600.
As preferably, in step (1), the temperature of esterification is 130～150 DEG C, and the time of esterification is 8～10 littleTime, vacuum >=-0.08Mpa when esterification;
In step (2), the temperature of sulfonating reaction is 80～110 DEG C, and the time of sulfonating reaction is 4～6 hours;
In step (3), the reaction temperature of esterification is 130～150 DEG C, and the reaction time of esterification is 6～8 littleTime, vacuum >=-0.08Mpa when esterification.
Therefore, the synthesis preparation method of a kind of Superfine Fibre Fabric high temperature levelling agent of the present invention, better permeance property,Therefore can make dyestuff be penetrated into comparatively easily superfine fibre inside under the effect of levelling agent to play the effect of level dyeing.
Brief description of the drawings
Fig. 1 is the infrared spectrogram of the A component of embodiment 1 in the present invention;
Fig. 2 is the infrared spectrogram of the B component of embodiment 2 in the present invention;
Fig. 3 is the infrared spectrogram of the C component of embodiment 3 in the present invention.
Detailed description of the invention
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1: a kind of synthesis preparation method of Superfine Fibre Fabric high temperature levelling agent, carries out according to the following steps:
(1), the preparation of high temperature levelling agent A component:
In the stainless steel cauldron of 1000L, add successively aliphatic acid and polyethylene glycol, under strong acid catalyst effect, enterRow esterification, the synthetic high temperature levelling agent A component that obtains; Described aliphatic acid and the ratio of the amount of substance of polyethylene glycol be 1 ~2:1, the amount of described strong acid catalyst is 0.5 ~ 1% of aliphatic acid and polyethylene glycol quality summation, described reaction temperature is 130 ~150 DEG C, the described reaction time is 8 ~ 10 hours, vacuum >=-0.08Mpa.
Following table is that high temperature levelling agent A component is respectively implemented reaction condition:
Considerable by Fig. 1: the peak of wave number 1734.15 represent polyunsaturated fatty acid ester-C=O absworption peak, illustrate and synthesized ester classComponent, infrared spectrum shows that the product structure of embodiment 1 is consistent with the object construction of A component.
(2), the preparation of high temperature levelling agent B component:
In the stainless steel cauldron of 500L, phenol APEO and urea, sulfamic acid are carried out to sulfonating reaction,To high temperature levelling agent B component; The ratio of the amount of substance of described phenol APEO and urea, sulfamic acid be 1:0.25 ~0.5:0.5 ~ 1, reaction temperature is 80 ~ 110 DEG C, 4 ~ 6 hours reaction time.
Following table is that high temperature levelling agent B component is respectively implemented reaction condition:
Considerable by Fig. 2: wave number is the deformation vibration of 1240.30,1172.99,1153.58,1044.18 represent-S=O of peakAbsworption peak, the deformation vibration small peak of represent-S=O of the peak that wave number is 690.34, the product structure that infrared spectrum shows embodiment 1 withThe object construction of B component is consistent.
(3), the preparation of high temperature levelling agent C component:
In the stainless steel cauldron of 1000L, add successively adipic acid and poly glycol monomethyl ether, do at strong acid catalystWith under carry out esterification, the synthetic high temperature levelling agent C component that obtains; Described adipic acid and the material of poly glycol monomethyl etherThe ratio of amount is 1:2, and the amount of described strong acid catalyst is 0.5 ~ 1% of adipic acid and poly glycol monomethyl ether quality summation, instituteStating reaction temperature is 130 ~ 150 DEG C, and the described reaction time is 6 ~ 8 hours, vacuum >=-0.08Mpa.
Following table is that high temperature levelling agent C component is respectively implemented reaction condition:
Considerable by Fig. 3: the peak that wave number is 1731.83 represent polyunsaturated fatty acid ester class-C=O absworption peak, illustrate effectively and closeBecome ester class component, infrared spectrum shows that the product structure of embodiment 1 is consistent with the object construction of C component.
(4), high temperature levelling agent is composite
After high temperature levelling agent A component, B component and C component is composite by the raw material of following weight portion, be high temperature level dyeingAgent:
20 ~ 62 parts of high temperature levelling agent A components
6 ~ 18 parts of high temperature levelling agent B components
4 ~ 10 parts of high temperature levelling agent C components
5 ~ 10 parts of isopropyl alcohols
15 ~ 65 parts, water
Following table is composite embodiment:
High temperature levelling agent A component, high temperature levelling agent B component, high temperature levelling agent C component are added in reactor successively, riseTemperature is to 60～70 degree, and the time of stirring is 30 minutes, adds water and opens cooling water and lower the temperature, when temperature is down to 30～40 degreeTime, close cooling water, then add isopropyl alcohol, then stir discharging 15 minutes.
Levelling agent contrasts for the situation of permeance property:
After being converted to 100% according to solid content, self-control levelling agent, conventional levelling agent be mixed with again
1% 200 milliliters of the aqueous solution, measure time of penetration with standard canvas and (put into and start timing to canvas from canvasBeing sink to bottom finishes).
Experimental data:
Application experiment situation:
1, experiment material:
20CM × 20CM superfine fibre woven dacron, self-control levelling agent, glacial acetic acid, disperse dyes, glass bar, SandoLab are completeCan try look experimental machine, Color-Eye7000A colour photometer.
2, experimental technique method "
2.1 slow metachromias
Red-1 200 .2%, disperse yellow 0.9%, dispersion blue 2.4% and levelling agent (are contained solid
Amount conversion is to 20%) 1g/L, bath raio 1:15, adds glacial acetic acid to regulate pH=5-5.5, controls 1 DEG C/point of programming rateClock, the slow metachromia of sampling and testing after dyeing in 90 DEG C × 10 minutes, 110 DEG C × 10 minutes, 130 DEG C × 30 minutes.
Experimental data:
2.2 achromicities:
To disperse emerald green orchid 0.7%, disperse yellow 0.05% and levelling agent (solid content converts 20%) 1g/L, bath raio 1:15, addsEnter glacial acetic acid and regulate pH=5-5.5, control 1 DEG C/min of programming rate, after dyeing in 130 DEG C × 30 minutes, sampling and testing disappearsLook.
Experimental data:
2.3 migration properties:
The employing of fetching from dye-works is disperseed to superfine fibre cloth the moving as unification black 4% dyeing
Dye cloth, will be moved and dye cloth and move that dying cloth is stitched together and move and dye experiment, levelling agent 1g/L, bath raio 1:15, usesGlacial acetic acid regulates pH=5-5.5, controls 1 DEG C/min of programming rate, moves and dyes in 130 DEG C × 30 minutes sampling and testings that dyeProperty.
Experimental data:
2.4 dispersivenesses:
By dispersed ruby 0.3g/L, levelling agent (solid content converts 20%) 1g/L and working solution 100
Milliliter, regulates pH=5-5.5 with glacial acetic acid, controls 1 DEG C/min of programming rate, gets dye liquor in 130 DEG C × 30 minutesAfter 100 milliliters of suction filtrations, filter paper is dried, observe filter paper surface dye liquor spread condition, and evaluate rank, 1 grade the poorest, and 5 grades best.
Experimental data:
Claims (2)
1. a synthesis preparation method for Superfine Fibre Fabric high temperature levelling agent, is characterized in that carrying out according to the following steps:
(1), high temperature levelling agent A component is synthetic:
Taking aliphatic acid and polyethylene glycol as raw material, under strong acid catalyst effect, carry out esterification, syntheticly obtain high temperature level dyeingAgent A component;
Aliphatic acid is 1～2:1 with the ratio of the amount of substance of polyethylene glycol;
The amount of strong acid catalyst is 0.5%～1% of aliphatic acid and polyethylene glycol quality summation;
(2), high temperature levelling agent B component is synthetic:
Phenol APEO, urea and sulfamic acid are carried out to sulfonating reaction, obtain high temperature levelling agent B component;
The ratio of the amount of substance of phenol APEO, urea and sulfamic acid is 1:0.25～0.5:0.5～1;
(3), high temperature levelling agent C component is synthetic:
Adipic acid and poly glycol monomethyl ether are carried out to esterification under strong acid catalyst effect, the synthetic high temperature levelling agent that obtainsC component;
The ratio of the amount of substance of adipic acid and poly glycol monomethyl ether is 1:2;
The amount of strong acid catalyst is 0.5～1% of adipic acid and poly glycol monomethyl ether quality summation;
(4), composite: by the preparing burden by weight of the high temperature levelling agent in above each step:
20～62 parts of high temperature levelling agent A components
6～18 parts of high temperature levelling agent B components
4～20 parts of high temperature levelling agent C components
5～10 parts of isopropyl alcohols
15～65 parts, water
High temperature levelling agent A component, high temperature levelling agent B component, high temperature levelling agent C component are added in reactor successively, be warming up to60～70 degree, the time of stirring is 30 minutes, adds water and opens cooling water and lower the temperature, when temperature is down to 30～40 while spending,Close cooling water, then add isopropyl alcohol, then stir discharging 15 minutes;
Described aliphatic acid is any one in isooctyl acid, different n-nonanoic acid and isodecyl acid;
The molecular size range of described polyethylene glycol is 400～800;
Described strong acid catalyst is DBSA;
The EO number of described phenol APEO is 3～7;
In described poly glycol monomethyl ether structure, molecular weight polyethylene glycol is 200～600.
2. the synthesis preparation method of a kind of Superfine Fibre Fabric high temperature levelling agent according to claim 1, is characterized in that:
In step (1), the temperature of esterification is 130～150 DEG C, and the time of esterification is 8～10 hours, when esterificationVacuum >=-0.08Mpa;
In step (2), the temperature of sulfonating reaction is 80～110 DEG C, and the time of sulfonating reaction is 4～6 hours;
In step (3), the reaction temperature of esterification is 130～150 DEG C, and the reaction time of esterification is 6～8 hours, esterVacuum >=-0.08Mpa while changing reaction.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105648797A (en) * | 2016-04-12 | 2016-06-08 | 湖州吉昌丝绸有限公司 | Environment-friendly and efficient biparental levelling agent |
| CN106436376B (en) * | 2016-09-19 | 2019-03-19 | 江苏工程职业技术学院 | A kind of preparation method of polyester-cotton fabric co-bathing dyeing levelling agent |
| CN107841894A (en) * | 2017-10-18 | 2018-03-27 | 马多浩 | A kind of water-based levelling agent of superfine fiber synthetic leather dyeing |
| CN108642919B (en) * | 2018-05-06 | 2020-06-19 | 安徽丽达制衣有限公司 | Special high-temperature leveling agent for superfine fiber fabric |
| CN108729266A (en) * | 2018-05-07 | 2018-11-02 | 浙江科峰新材料有限公司 | A kind of preparation method of alkalinity high temperature levelling agent |
| CN110015957A (en) * | 2019-03-30 | 2019-07-16 | 镇江巨杰新材料技术研发中心(有限合伙) | A kind of synthetic method and application of polyethylene glycol 400 tricaprylate |
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