CN102011317A - High-alkali-resistance wet cloth silkete penetrating agent and preparation method thereof - Google Patents
High-alkali-resistance wet cloth silkete penetrating agent and preparation method thereof Download PDFInfo
- Publication number
- CN102011317A CN102011317A CN 201010527958 CN201010527958A CN102011317A CN 102011317 A CN102011317 A CN 102011317A CN 201010527958 CN201010527958 CN 201010527958 CN 201010527958 A CN201010527958 A CN 201010527958A CN 102011317 A CN102011317 A CN 102011317A
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- China
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- penetrating agent
- wet cloth
- polyoxyethylene ether
- preparation
- deionized water
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Abstract
The invention discloses a high-alkali-resistance wet cloth silkete penetrating agent and a preparation method thereof. The penetrating agent is Lutensol TO phosphate. Compared with the prior art, the high-alkali-resistance wet cloth silkete penetrating agent has high alkali resistance, high biodegradability, excellent wettability and emulsification performance and no side or toxic effect, and can be widely mixed with other auxiliary agents. The high-alkali-resistance penetrating agent is synthesized by a phosphorus pentoxide direct phosphating method, so the preparation method is simple in operation and mild in reaction condition. The developed high-alkali-resistance wet cloth silkete penetrating agent can be applied to the wet cloth mercerizing process of cotton, linen fabric and blend fabric of the cotton and the line fabric.
Description
Technical field
The invention belongs to printing and dyeing assistant and preparation method thereof, belong to bleeding agent and preparation method thereof especially.
Background technology:
Mercerising can improve the absorption property and the glossiness of fabric, improves the DIMENSIONAL STABILITY of fabric, is important step in the fabric finishing pre-treatment.In the conventional dried cloth mercerization of fabric, can only realize surperficial mercerising because the infiltration of alkali lye is insufficient, mercerization effect is undesirable, needs that cloth is carried out drying before the mercerising simultaneously to obtain dried cloth, expends a large amount of energy.The wet cloth mercerization of fabric can improve the permeability of mercerising alkali lye easy and significantly, can reduce the drying flow process in the pre-treatment process simultaneously, energy savings.In wet cloth mercerising, the alkali concn of mercerising treatment fluid is higher than 300g/l, because concentration of lye is higher, be thick at low temperatures, and the mercerising process time is of short duration, is unfavorable for that alkali lye can enter fabric fibre inside fast, is difficult to obtain desirable mercerization effect.For improving the mercerising product quality, obtain uniform mercerization effect, should in mercerising liquid, add mercerizing assistant, because concentration of lye is higher than traditional mercerization in the wet cloth mercerization, mercerizing assistant commonly used not resisting high-concentration alkali (〉=280g/l), limited the promotion and application of wet cloth mercerization.
Summary of the invention
The 1st technical problem to be solved by this invention provides a kind of high alkaline-resisting wet cloth silkete penetrating agent.
The 2nd technical problem to be solved by this invention is the preparation method of above-mentioned silkete penetrating agent.
The technical scheme of technical solution problem of the present invention is: a kind of high alkaline-resisting wet cloth silkete penetrating agent, described bleeding agent is the isomerous tridecanol polyoxyethylene ether phosphate.
Described isomerous tridecanol polyoxyethylene ether phosphate comprises (RO-(C
2H
4O) n)
2PO (OH) (MAP), RO-(C
2H
4O) n PO (OH) (DAP), (RO-(C
2H
4O) n)
2PO (OH) (MAP) with RO-(C
2H
4O) n PO (OH) mol ratio (DAP) is (15-22): 1;
Described n=7-10;
Described R is different tridecanol: molecular formula: C
13H
28O;
Structural formula: CH
3-CH (CH
3)-CH
2-CH
2-CH
2-CH
2-CH
2-CH
2-CH
2-CH
2-CH
2-CH
2-OH.
Preparation method of the present invention is:
A, esterification step: isomerous tridecanol polyoxyethylene ether is added in the deionized water, be warmed up to 70-100 ℃, under the situation that stirs, add P in batches
2O
5, after adding, be incubated 1-4 hour, obtain esterification products, isomerous tridecanol polyoxyethylene ether, deionized water, P
2O
5Mol ratio be 3: 0.6-1.5: 0.8-1.5;
B, hydrolyzing process: esterification products being added the deionized water hydrolysis 1-5 hour, cool to below 50 ℃, is 6～8 with aqueous slkali neutralising phosphoric acid ester to the pH value, gets final product, and the mol ratio of the deionized water in isomerous tridecanol polyoxyethylene ether and the hydrolysis is 3: 0.6-1.5.
Described aqueous slkali is that weight concentration is NaOH, the potassium hydroxide solution of 300-320g/l.
Preferred esterification step is: 90 ℃ of esterification temperatures, and esterification time 4h drops into phosphorus pentoxide in batches under the strong agitation, and the mol ratio of isomerous tridecanol polyoxyethylene ether, phosphorus pentoxide, deionized water is 3: 1: 1.
Preferred hydrolyzing process is: 90 ℃ of hydrolysis temperatures, and hydrolysis time 3 hours, the mol ratio of isomerous tridecanol polyoxyethylene ether, deionized water is 3: 1.
Reaction principle of the present invention is:
4RO(CH
2CH
2O)
nH+P
2O
5——2[RO(CH
2CH
2O)
n]
2PO(OH)+H
2O
2RO(CH
2CH
2O)
nH+P
2O
5+H
2O——2RO(CH
2CH
2O)
nPO(OH)
2
3RO(CH
2CH
2O)
nH+P
2O
5——[RO(CH
2CH
2O)
n]2PO(OH)+RO(CH
2CH
2O)
nPO(OH)
2
Because phosphate monoester has two-O-group in aqueous slkali, water-soluble and alkali resistance all is higher than phosphate diester, but the surface tension of phosphate monoester solution and critical micelle concentration be all greater than phosphate diester, so the permeability phosphate monoester is not as phosphate diester.Therefore, the alkali resistance of phosphate and permeability are conflicting, for the phosphate of synthetic high alkaline-resisting high osmosis, must realize by adjusting single dibasic acid esters ratio.
The present invention compared with prior art, act in the 300g/L sodium hydroxide solution, the wetting time of standard canvas is less than 5s, sedimentation time is less than 10s, have good anti-highly basic penetrating power, and an alkali lye clarification, and improve the absorption property of mercerizing barium value, fabric, lower the broadwise washing shrinkage of fabric, mercerising is handled evenly; Simultaneously because wet cloth mercerising all carries out the dyeing and finishing pre-treatment of fabric under hygrometric state; can not only keep the fabric work in-process to have higher flexibility and adsorptivity; avoided pilot process trace impurity, alkaline agent etc. in drying process, to concentrate the infringement that dyeing and finishing quality is caused, thereby protected the style of fabric and improve the dyeing and finishing effect.
The specific embodiment
Below in conjunction with embodiment the present invention is done detailed explanation.
Embodiment 1:
A, esterification step: isomerous tridecanol polyoxyethylene ether (commercially available) is added in the deionized water, under the situation that stirs, add P in batches
2O
5, after adding, be warmed up to 90 ℃, be incubated 4 hours, obtain esterification products, isomerous tridecanol polyoxyethylene ether, deionized water, P
2O
5Mol ratio be 3: 1: 1;
B, hydrolyzing process: esterification products being added the deionized water hydrolysis 3 hours, cool to below 50 ℃, is 7 with the sodium hydroxide solution neutralising phosphoric acid ester of 0.1M to the pH value, gets final product, and the mol ratio of the deionized water in isomerous tridecanol polyoxyethylene ether and the hydrolysis is 3: 1.
(RO-(the C that makes
2H
4O) n)
2PO (OH) (MAP), RO-(C
2H
4O) n PO (OH) (DAP), (RO-(C
2H
4O) n)
2PO (OH) (MAP) with RO-(C
2H
4O) n PO (OH) (DAP) mol ratio be 22: 1;
Described n=8;
Embodiment 2:
Remove in a, the esterification step isomerous tridecanol polyoxyethylene ether (ROH), P
2O
5The mol ratio difference outside, all the other are identical with embodiment 1, its result is as shown in table 1:
Table 1:
As shown in Table 1: isomerous tridecanol polyoxyethylene ether there are differences with single, double ester content and ratio thereof that phosphorus pentoxide is surveyed in different proportioning, and wetting time, the sedimentation time of the solution of anti-300g/LNaOH also have nothing in common with each other.Along with the increase of proportioning, the ratio of phosphate diester decrescence, but the ratio of monoesters and dibasic acid esters increases gradually.The sedimentation time of standard canvas reduces gradually with the increase of MAP: DAP, and the basic no change of its alkali resistance.When proportioning was 6: 1 and 5: 1, the wetting time of sintetics was very short, but the standard canvas sedimentation time is very long, not even sedimentation.This is because under this proportioning, fatty alcohol ether is excessive, causes the fatty alcohol ether that has unreacted intact in the product, and it floats on the alkali lye surface when test, so the standard canvas of making is very easily wetting, but because it can't make alkali lye permeate in fiber, so the not sedimentation of standard canvas.Wetting time, the sedimentation time of synthetic sample under comprehensive relatively each proportioning, select to be decided to be at 3: 1 optimum charging ratio.The permeability of product and alkali resistance the best under this rate of charge.
Embodiment 3:
The temperature difference in a, esterification step, all the other are identical with embodiment 1, its result such as table 2.
Table 2:(300g/L sodium hydroxide solution, 3% phosphate)
Because temperature is very important process conditions to organic synthesis, temperature is low excessively, and then reaction speed is too slow, and esterification is incomplete; Improve temperature, reaction speed is accelerated, but the harmful effect of following two aspects of the too high easy generation of Phosphation temperature easily produces the dehydration etherificate between hydroxyl, and hydroxy radical content is reduced; Esterification reaction temperature raises and also can impel esterification reaction rate to increase, but can produce more accessory substance, and product color is deepened.
As shown in Table 2, along with the lifting of esterification temperature, the ratio of monoesters and dibasic acid esters increases gradually in the synthetic phosphoric acid ester, and the wetting time of sintetics, sedimentation time all successively decrease, and this shows that the lifting of esterification temperature helps the alkaline-resisting permeance property of synthetic phosphoric acid ester product.Because the alkaline-resisting permeability of 90 ℃ of products is best, so esterification reaction temperature is decided to be 90 ℃.
Embodiment 4:
The reaction time difference in a, esterification step, all the other are identical with embodiment 1, and its result such as table 3 are not.
Table 3
Because phosphorus pentoxide is a solid, be extremely difficult from the initial reaction stage analysis that comprises the phosphorus pentoxide course of dissolution, when inquiring into esterification time, esterification time is that homogeneous phase picks up counting from reactant liquor.As shown in Table 3: after autoreaction liquid becomes homogeneous phase, reaction time is less to the content influence of free phosphoric acid in esterification yield and the reaction system, but along with the increase phosphate monoester content in reaction time increases, and phosphate diester content reduces, esterification time reacted in the time of 4 hours and reaches balance substantially, and single dibasic acid esters ratio is the highest in the product, and indexs such as the wetting time of comprehensive product, sedimentation time are best esterification time so select 4 hours.
Embodiment 5:
Remove in b, the hydrolyzing process, add the water mode and can be divided into and once add water, hydrolysis before the hydrolysis and add water in batches, do not add three kinds of technologies of water, its result is as shown in table 4:
Table 4
As shown in Table 4: disposablely before hydrolysis add the hydrolysis that water helps polyphosphate, so select the disposable water conservancy project skill that adds before the hydrolysis;
Embodiment 6:
Remove in b, the hydrolyzing process, outside the hydrolysis time difference, all the other are identical with embodiment 1, and its result is as shown in table 5:
Table 5
As shown in Table 5: with
Between prolongation, the ratio of monoesters is listed in increase, from MAP/DAP than the row as can be known, when hydrolysis reached 3h, hydrolysis reached balance substantially, so definite hydrolysis time is 3h.
Embodiment 7:
(move back behind the boiling and bleaching process dry the wet fabric of cotton, liquid carrying rate is 80%) tight placing on the tension bracket, and fabric is dipped in the concentrated caustic solution that concentration is 300g/l, mercerizing assistant concentration is 2g/l, pad mercerising liquid, pick-up rate is 110%, mercerising after the hot water injection, fully cold wash to neutral, dry.Fabric carries out the mercerising test according to experimental condition, adopts unified washing lixiviating mode to wash, dry behind the mercerising, and absorption property, the powerful index of mercerising processing fabric are carried out test analysis.And carry out the test comparison of brute force and barium value with the dried cloth mercerized cloth of routine, result of the test sees the following form shown in 1:
Wet cloth mercerising performance test of table 1. fabric and contrast
Compare with conventional mercerized cloth, the brute force of fabric increases behind the wet cloth mercerising, and reason is that fabric namely enters mercerization under hygrometric state, reduced the damage of flint dry to fabric strength; On the other hand, in the wet cloth mercerising technology, alkali lye has improved the permeance property of alkali lye to fabric under the effect of additive synthesis isomerous tridecanol polyoxyethylene ether phosphate, and mercerization finish is even, is conducive to improve the degree of orientation of fiber, reduces the damage to fabric strength. Simultaneously, wet cloth mercerising technology can improve the mercerizing barium value of fabric, increases the absorption property of fabric, lowers the broadwise washing shrinkage of fabric, guarantees the dimensional stability of fabric.
Claims (6)
1. one kind high alkaline-resisting wet cloth silkete penetrating agent, it is characterized in that: described bleeding agent is the isomerous tridecanol polyoxyethylene ether phosphate.
2. a kind of high alkaline-resisting wet cloth silkete penetrating agent according to claim 1, it is characterized in that: described isomerous tridecanol polyoxyethylene ether phosphate comprises (RO-(C
2H
4O) n)
2PO (OH), RO-(C
2H
4O) n PO (OH), (RO-(C
2H
4O) n)
2PO (OH) and RO-(C
2H
4O) mol ratio of n PO (OH) is (15-22): 1;
Described n=7-10;
Described R is different tridecanol.
3. the preparation method of the described a kind of high alkaline-resisting wet cloth silkete penetrating agent of claim 1 is characterized in that: comprise following operation:
A, esterification step: isomerous tridecanol polyoxyethylene ether is added in the deionized water, be warmed up to 70-100 ℃, under the situation that stirs, add P in batches
2O
5, after adding, be incubated 1-4 hour, obtain esterification products, isomerous tridecanol polyoxyethylene ether, deionized water, P
2O
5Mol ratio be 3: 0.6-1.5: 0.8-1.5;
B, hydrolyzing process: esterification products being added the deionized water hydrolysis 1-5 hour, cool to below 50 ℃, is 6～8 with aqueous slkali neutralising phosphoric acid ester to the pH value, gets final product, and the mol ratio of the deionized water in isomerous tridecanol polyoxyethylene ether and the hydrolysis is 3: 0.6-1.5.
4. the preparation method of a kind of high alkaline-resisting wet cloth silkete penetrating agent according to claim 3 is characterized in that: described aqueous slkali is that weight concentration is NaOH, the potassium hydroxide solution of 300-320g/l.
5. the preparation method of a kind of high alkaline-resisting wet cloth silkete penetrating agent according to claim 3, it is characterized in that: described esterification step is: 90 ℃ of esterification temperatures, esterification time 4 hours, drop into phosphorus pentoxide under the strong agitation, the mol ratio of isomerous tridecanol polyoxyethylene ether, phosphorus pentoxide, deionized water is 3: 1: 1 in batches.
6. the preparation method of a kind of high alkaline-resisting wet cloth silkete penetrating agent according to claim 3 is characterized in that: preferred hydrolyzing process is: 90 ℃ of hydrolysis temperatures, and hydrolysis time 3 hours, the mol ratio of isomerous tridecanol polyoxyethylene ether, deionized water is 3: 1.
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|---|---|---|---|
| CN 201010527958 CN102011317B (en) | 2010-11-01 | 2010-11-01 | High-alkali-resistance wet cloth silkete penetrating agent and preparation method thereof |
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| CN102011317B CN102011317B (en) | 2012-07-18 |
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| CN102503973A (en) * | 2011-11-02 | 2012-06-20 | 浙江皇马科技股份有限公司 | Preparation method of a strong base-resistant mercerization penetrating agent of ethylene glycol monobutyl ether phosphate |
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| CN102653921A (en) * | 2012-04-26 | 2012-09-05 | 天津达一琦精细化工有限公司 | Alkali-resisting penetrating agent for cotton fabric mercerization |
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