CN102503973B - A kind of preparation method of the silkete penetrating agent of resistance to highly basic butyl glycol ether phosphoric acid ester - Google Patents
A kind of preparation method of the silkete penetrating agent of resistance to highly basic butyl glycol ether phosphoric acid ester Download PDFInfo
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- CN102503973B CN102503973B CN201110340635.2A CN201110340635A CN102503973B CN 102503973 B CN102503973 B CN 102503973B CN 201110340635 A CN201110340635 A CN 201110340635A CN 102503973 B CN102503973 B CN 102503973B
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- glycol ether
- butyl glycol
- phosphoric acid
- acid ester
- ether phosphoric
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Abstract
The invention discloses a kind of preparation method of the silkete penetrating agent of resistance to highly basic butyl glycol ether phosphoric acid ester, carry out phosphorylation reaction with butyl glycol ether and polyphosphoric acid, then add deionized water hydrolysis, obtain butyl glycol ether phosphoric acid ester; Described butyl glycol ether phosphoric acid ester, mainly comprises phosphate monoester MAP and phosphate diester DAP; The general formula of described polyphosphoric acid is: H
n+2p
no
3n+1; Polymerization degree n=3 ~ 6; The amount mol ratio of described polyphosphoric acid and butyl glycol ether is 1:1 ~ 7.The present invention, under concentrated base condition, can not produce ammonia taste and foam, does not affect the recovery of alkali lye; The alkali charge of all mercerizations can be met; Have reaction temperature and, technique is simple, stable, and easily control, facility investment is little, the feature of high financial profit.
Description
Technical field
The present invention relates to a kind of preparation method of the silkete penetrating agent of resistance to highly basic butyl glycol ether phosphoric acid ester, belong to the synthesis technical field of anion surfactant in organic chemistry.
Background technology
As the necessary resistance to highly basic of silkete penetrating agent, environmental pollution is little.And phosphoric acid ester is that a class cloud point is high, the high-efficient penetrant of resistance to highly basic, high temperature resistant, nontoxic, low bubble, readily biodegradable, development in recent years is very fast, and in pretreatment of spinning, such variety development is more, applies wider.During cotton fabric mercerising, because the speed of a motor vehicle is fast, easily produce foam; In addition, because the strong basicity of mercerising liquid and higher ionic strength may cause permeate agent destroy or saltout; Require when mercerized waste alkali reclaims that permeate agent not easily decomposes in the process, foam is little, does not affect the recovery process of light alkali.Consider above factor, therefore phosphoric acid ester hydrophobic group should not more than 8 carbon atoms.Because phosphate monoester has 2-O in alkaline solution
-group, good water solubility, alkali resistance, also higher than phosphate diester, requires that the phosphate monoester selected that alkali resistance is high is major product; The phosphate diester of then selecting of requirement good penetrability is major product.Therefore, the phosphoric acid ester working out a kind of single, double ester content of low carbon chain of the silkete penetrating agent of resistance to highly basic suitable is significant.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of the silkete penetrating agent of resistance to highly basic butyl glycol ether phosphoric acid ester, the present invention, under concentrated base condition, can not produce ammonia taste and foam, does not affect the recovery of alkali lye; The alkali charge of all mercerizations can be met; Have reaction temperature and, technique is simple, stable, and easily control, facility investment is little, the feature of high financial profit.
In order to achieve the above object, technical scheme of the present invention is:
A preparation method for the silkete penetrating agent of resistance to highly basic butyl glycol ether phosphoric acid ester, carries out phosphorylation reaction with butyl glycol ether and polyphosphoric acid, then adds deionized water hydrolysis, obtains butyl glycol ether phosphoric acid ester; Described butyl glycol ether phosphoric acid ester, mainly comprise phosphate monoester MAP and phosphate diester DAP, structural formula is respectively:
The general formula of described polyphosphoric acid is: H
n+2p
no
3n+1; Polymerization degree n=3 ~ 6; The amount mol ratio of described polyphosphoric acid and butyl glycol ether is 1:1 ~ 7.
Described phosphorylation reaction temperature is 60 ~ 90 DEG C, and the reaction times is 2 ~ 6 hours.
Described hydrolysis temperature is 70 ~ 90 DEG C, and the reaction times is 0.5 ~ 2.0 hour, and the add-on of deionized water is 0.5 ~ 3% of butyl glycol ether and polyphosphoric acid total mass.
The invention has the beneficial effects as follows: (1) hydrophobic group is less than the phosphoric acid ester silkete penetrating agent of the butyl glycol ether synthesis of 8 carbon atoms, under concentrated base condition, can not produce ammonia taste and foam, not affect the recovery of alkali lye.
(2) polyphosphoric acid substitutes Vanadium Pentoxide in FLAKES as phosphoric acid agent, can synthesize the phosphoric acid ester that monoester content is higher, increases its alkali resistance, and normal temperature is alkaline-resisting can reach 300g/L, can meet the alkali charge of all mercerizations.
(3) polyphosphoric acid is as phosphoric acid agent, reaction temperature and, technique is simple, stable, and easily control, facility investment is little, high financial profit.
Embodiment
Embodiment 1
1000.0mol(118.0kg is added in enamel reaction still) butyl glycol ether, slowly evenly add 1000.0mol(418.0kg) polyphosphoric acid of polymerization degree n=5, control temperature is no more than 55 DEG C.Add polyphosphoric acid, be warming up to 60 ~ 62 DEG C, insulation reaction 6.0 hours.Insulation is finished, and is warming up to 80 ~ 82 DEG C, adds 16.1kg deionized water, be hydrolyzed 2.0 hours, and cooling, obtains sample butyl glycol ether phosphoric acid ester.The present embodiment product, under concentrated base condition, can not produce ammonia taste and foam, does not affect the recovery of alkali lye; The alkali charge of all mercerizations can be met; Have reaction temperature and, technique is simple, stable, and easily control, facility investment is little, the feature of high financial profit.
Embodiment 2
7000.0mol(826.0kg is added in enamel reaction still) butyl glycol ether, slowly evenly add 1000.0mol(498.0kg) polyphosphoric acid of polymerization degree n=6, control temperature is no more than 55 DEG C.Add polyphosphoric acid, be warming up to 88 ~ 90 DEG C, insulation reaction 2.0 hours.Insulation is finished, and is cooled to 70 ~ 72 DEG C, adds 6.6kg deionized water, be hydrolyzed 1.0 hours, and cooling, obtains sample butyl glycol ether phosphoric acid ester.The present embodiment product, under concentrated base condition, can not produce ammonia taste and foam, does not affect the recovery of alkali lye; The alkali charge of all mercerizations can be met; Have reaction temperature and, technique is simple, stable, and easily control, facility investment is little, the feature of high financial profit.
Embodiment 3
4000.0mol(472.0kg is added in enamel reaction still) butyl glycol ether, slowly evenly add 1000.0mol(338.0kg) polyphosphoric acid of polymerization degree n=4, control temperature is no more than 55 DEG C.Add polyphosphoric acid, be warming up to 80 ~ 82 DEG C, insulation reaction 4.0 hours.Insulation is finished, and is warming up to 88 ~ 90 DEG C, adds 16.2kg deionized water, be hydrolyzed 0.5 hour, and cooling, obtains sample butyl glycol ether phosphoric acid ester.The present embodiment product, under concentrated base condition, can not produce ammonia taste and foam, does not affect the recovery of alkali lye; The alkali charge of all mercerizations can be met; Have reaction temperature and, technique is simple, stable, and easily control, facility investment is little, the feature of high financial profit.
Embodiment 4
5000.0mol(590.0kg is added in enamel reaction still) butyl glycol ether, slowly evenly add 1000.0mol(258.0kg) polyphosphoric acid of polymerization degree n=3, control temperature is no more than 55 DEG C.Add polyphosphoric acid, be warming up to 70 ~ 72 DEG C, insulation reaction 3.0 hours.Insulation is finished, and is warming up to 75 ~ 77 DEG C, adds 14.8kg deionized water, be hydrolyzed 1.5 hours, and cooling, obtains sample butyl glycol ether phosphoric acid ester.The present embodiment product, under concentrated base condition, can not produce ammonia taste and foam, does not affect the recovery of alkali lye; The alkali charge of all mercerizations can be met; Have reaction temperature and, technique is simple, stable, and easily control, facility investment is little, the feature of high financial profit.
Embodiment 5
2000.0mol(236.0kg is added in enamel reaction still) butyl glycol ether, slowly evenly add 1000.0mol(338.0kg) polyphosphoric acid of polymerization degree n=4, control temperature is no more than 55 DEG C.Add polyphosphoric acid, be warming up to 85 ~ 87 DEG C, insulation reaction 5.0 hours.Insulation is finished, and is cooled to 83 ~ 85 DEG C, adds 5.7kg deionized water, be hydrolyzed 1.0 hours, and cooling, obtains sample butyl glycol ether phosphoric acid ester.The present embodiment product, under concentrated base condition, can not produce ammonia taste and foam, does not affect the recovery of alkali lye; The alkali charge of all mercerizations can be met; Have reaction temperature and, technique is simple, stable, and easily control, facility investment is little, the feature of high financial profit.
Sample butyl glycol ether phosphoric acid ester prepared by embodiment 1-5, single, double ester content, alkaline-resisting seepage force, alkali resistance are as shown in table 1.As can be seen from Table 1, in sample, single, double ester content one timing, has best alkaline-resisting seepage force.
Embodiment 6
The effect measuring (barium value method) of mercerising
All-cotton fabric (boiling drift through moving back) the one alkali immerging one ventilative alkali immerging one of cloth that stretches tight neutralizes a washing
Mangle expression: 70 ~ 80%, concentration of lye 300g/L, butyl glycol ether phosphoric acid ester 10g/L, lixiviating temperature 80 DEG C.
Barium value method be by mercerising after cotton and the cotton of non-mercerising immerse in barium hydroxide solution respectively and keep the regular hour, then the ratio that mercerising sample and non-mercerising sample adsorb hydrated barta is obtained, institute's value is barium value, and the adsorptivity of the larger expression mercerized fiber of barium value is better.
As shown in table 2, table 2 is cotton fabric mercerizing barium value test data table, from table 2 barium value test data result, the mercerizing barium value having added the butyl glycol ether phosphoric acid ester of the certain content of single, double ester is more much higher than the barium value do not added, therefore, can illustrate that the butyl glycol ether phosphoric acid ester of synthesis is a kind of silkete penetrating agent of resistance to highly basic well.
Claims (1)
1. the preparation method of the silkete penetrating agent of a resistance to highly basic butyl glycol ether phosphoric acid ester, it is characterized in that: carry out phosphorylation reaction with butyl glycol ether and polyphosphoric acid, 1000.0mol butyl glycol ether is added in enamel reaction still, slowly evenly add the polyphosphoric acid of 1000.0mol polymerization degree n=5, control temperature is no more than 55 DEG C; Add polyphosphoric acid, be warming up to 60 ~ 62 DEG C, insulation reaction 6.0 hours; Insulation is finished, and is warming up to 80 ~ 82 DEG C, adds 16.1kg deionized water, be hydrolyzed 2 hours, and cooling, obtains butyl glycol ether phosphoric acid ester; Described butyl glycol ether phosphoric acid ester mainly comprises phosphate monoester MAP and phosphate diester DAP, and the mass percent that the mass percent of MAP is 92.7%, DAP is 2.1%, and concrete structure formula is respectively:
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| CN103882504B (en) * | 2014-04-11 | 2016-03-23 | 武汉一枝花油脂化工有限公司 | A kind of grease-removing agent of silicate |
| CN109516623B (en) * | 2018-11-16 | 2021-06-01 | 浙江万盛股份有限公司 | Comprehensive utilization method of tributoxyethyl phosphate wastewater |
| CN114907238A (en) * | 2022-06-16 | 2022-08-16 | 淄博鲁瑞精细化工有限公司 | Alkyl alcohol polyoxyethylene ether sulfate salt for mercerizing penetrant and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125861A (en) * | 2007-07-24 | 2008-02-20 | 王伟松 | Method for synthesizing aliphatic alcohol polyoxyvinethene phosphate |
| CN101525330A (en) * | 2008-03-07 | 2009-09-09 | 上海医药工业研究院 | Phosphopyridoxal intermediates, preparation method of same, application of same, and method for preparing phosphopyridoxal therefrom |
| CN102011317A (en) * | 2010-11-01 | 2011-04-13 | 安徽工程大学 | High-alkali-resistance wet cloth silkete penetrating agent and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125861A (en) * | 2007-07-24 | 2008-02-20 | 王伟松 | Method for synthesizing aliphatic alcohol polyoxyvinethene phosphate |
| CN101525330A (en) * | 2008-03-07 | 2009-09-09 | 上海医药工业研究院 | Phosphopyridoxal intermediates, preparation method of same, application of same, and method for preparing phosphopyridoxal therefrom |
| CN102011317A (en) * | 2010-11-01 | 2011-04-13 | 安徽工程大学 | High-alkali-resistance wet cloth silkete penetrating agent and preparation method thereof |
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