Lignose alcohol ether carboxylate surfactant and preparation method thereof

A technology of alcohol ether carboxylate and surfactant, which is applied in the field of surfactant preparation, can solve the problem that the preparation method of alcohol ether carboxylate surfactant has not been reported, and can change serious environmental pollution and make full use of resources. Effect

Inactive Publication Date: 2008-12-24
JIANGSU QIANGLIN BIO ENERGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] But, the preparation method of using lignin to prepare alcohol ether carboxylate surfactant has not been reported

Method used

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  • Lignose alcohol ether carboxylate surfactant and preparation method thereof
  • Lignose alcohol ether carboxylate surfactant and preparation method thereof
  • Lignose alcohol ether carboxylate surfactant and preparation method thereof

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Experimental program
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preparation example Construction

[0033] Preparation of lignin alcohol ether:

[0034] In the first step, 100 parts by mass of purified lignin with a mass fraction of lignin above 95%, 0.1-5 parts by mass of the catalyst NaOH, 20-100 parts by mass of the solvent toluene, and reaction in an oxygen-free environment, the reaction temperature is 80-150°C, The reaction pressure is 0.3 to 1.0 MPa, stirring, and 10 to 100 parts by mass of ethylene oxide and 10 to 100 parts by mass of propylene oxide are divided into 2 to 10 groups;

[0035] In the second step, one group of ethylene oxide is introduced and reacted for 30-60 minutes each time, and then another group of propylene oxide is introduced to react for 30-60 minutes;

[0036] In the third step, repeat the second step until all the ethylene oxide and propylene oxide have reacted, stop the reaction and stop heating, stop stirring after cooling to room temperature, add inert gas to 1 atmosphere, and then distill under reduced pressure. The low boiling point fraction ...

Embodiment 1

[0038] The preparation method of lignin alcohol ether carboxylate is prepared by the following steps:

[0039] A base catalyst with 100 parts by mass of lignin alcohol ether and 1 to 1.2 times the amount of lignin alcohol ether is reacted at 90-110°C for 30-60 minutes, and low-boiling substances are removed under reduced pressure at -0.1MP, The amount of the added substance is 1.2 to 1.5 times of the halogenated acid of the lignin alcohol ether, and the reaction is carried out for 4 to 8 hours to obtain the lignin alcohol ether carboxylate.

[0040] The base catalyst can be 1, 1.1, 1.2 times the amount of lignin alcohol ether, the reaction temperature can be 90°C, 100°C, 110°C, the reaction time can be 30min, 45min, 60min, and the amount of halogenated acid can be It is 1.2 times, 1.35 times, 1.5 times, and the reaction time can be 4h, 5.5h, 8h. The halogenated acid can be any one of 2-chloropropionic acid, monochloroacetic acid, 2-bromopropionic acid, and bromoacetic acid; the al...

Embodiment 2

[0042] Preparation method of lignin alcohol ether carboxylate:

[0043] Add 100 parts by mass of the lignin alcohol ether and the catalyst NaOH in an amount 1.2 times the amount of the lignin alcohol ether, react at 90~100°C for 30 minutes, and then extract the water under reduced pressure, press the lignin alcohol ether and monochloroacetic acid Monochloroacetic acid was added dropwise in a molar ratio of 1:1.2, and reacted for 4 hours to obtain sodium salt of lignin alcohol ether carboxylate. Sampling to determine the hydroxyl value of the sodium salt of lignin alcohol ether carboxylate is 40 mg / g.

[0044] Comparison of IR spectrum analysis of lignin alcohol ether carboxylic acid sodium salt and raw material lignin alcohol ether: at 3700cm -1 ~3030cm -1 The absorption decreases, indicating that the hydroxyl group in the lignin alcohol ether is reacted, resulting in 3418.18cm -1 Absorption is reduced. . At 1096.25cm -1 The intensity of the absorption peak appears at the decrease...

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Abstract

The present invention discloses a lignin alcohol ether carboxylate novel surfactant preparation method. 100 weight proportions of lignin alcohol ether and base catalyst with 1 to 1.2 times of the weight proportions of the lignin alcohol ether react for 30 to 60 minutes under 90 to 110 DEG C; low-boiling substance is removed by decompressing under subtractive 0.1MP; halogenated acid with the substance quantity of 1.2 to 1.5 times of the lignin alcohol ether is added to react for 4 to 8 hours to obtain the lignin alcohol ether carboxylate. In the reaction steps, the lignin alcohol ether is prepared by self; the halogenated acid can be any one of 2-chloropropionic acid, chloroacetic acid, 2-bromo propionate or bromoacetic acid; the base catalyst is KOH or NaOH. In the characterization of the lignin alcohol ether carboxylate, foam performance water hardness is 150 multiplied by 10<subtractive 6>ppm as being measured by a Rockwell latherometer; sample content is 0.25 percent under 40 DEG C, the foam height is measured as the start height of 150mm; the foam height is 130mm after 5 minutes; when surface tension (delta) sample contents are 0.01 percent and 0.05 percent respectively, the surface tensions are respectively 57.2mN / m and 51.2mN / m; critical micelle concentration (CMC) measured value is 5.0g / L.

Description

Technical field [0001] The invention belongs to the field of surfactant preparation, and in particular relates to a preparation method of a new type of lignin alcohol ether carboxylate surfactant. Background technique [0002] At present, due to the shortage of petroleum resources and rising prices, the surfactant manufacturing industry is actively using natural renewable resources to produce products. Lignin, as a by-product of the wood hydrolysis industry and papermaking industry, has not been fully utilized and has become papermaking. One of the main sources of pollution in industry not only causes serious environmental pollution, but also causes a major waste of resources. Lignin is mainly composed of three elements: carbon, hydrogen, and oxygen. It is generally recognized that lignin is a cross-networked natural phenolic polymer compound composed of phenylpropyl (C9) units connected through C-0 bonds or C-C bonds. Because it contains a large number of phenolic hydroxyl...

Claims

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Application Information

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IPC IPC(8): B01F17/50C09K23/50
Inventor 周永红刘欣刘红军
Owner JIANGSU QIANGLIN BIO ENERGY
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