CN1151195C - Electrochemical process of preparing lignin in different molecular weight - Google Patents
Electrochemical process of preparing lignin in different molecular weight Download PDFInfo
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- CN1151195C CN1151195C CNB001310011A CN00131001A CN1151195C CN 1151195 C CN1151195 C CN 1151195C CN B001310011 A CNB001310011 A CN B001310011A CN 00131001 A CN00131001 A CN 00131001A CN 1151195 C CN1151195 C CN 1151195C
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- lignin
- molecular weight
- xylogen
- different molecular
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Abstract
The present invention relates to a preparation method of lignin with different molecular weights with an electrochemical method. The lignin is polymerized and degraded by controlling electric consumption in an electrochemical reaction carried out in a purpose-made reactor. Voltage of 2 to 13v is exerted on a certain amount of lignin during the reaction, the pH value of a solution is from 2 to 3, the time is from 1 to 90 hours, and reaction products can be used for synthesizing a surface active agent, a dye dispersing agent and a cement dispersing agent which have superior performance and can also be used as raw materials for synthetic resin. Compared with the existing chemical method and the existing thermochemical method, the method of the present invention has the advantages of mild reaction conditions, no need of the addition of a catalyst or other chemical reagents, no generation of public hazard, easy control of the molecular weights of the lignin, etc.
Description
The invention relates to electrochemical method and make the method for the xylogen of different molecular weight.
Xylogen is the general name that is present in the quasi-aromatic compound in the spermatophyte, is the natural polymer of a class formation complexity.Industrial xylogen all is alkali lignin or the sulfonated lignin of separating respectively in the waste black liquor (alkaline process and sulphate process papermaking wastewater) that produces from pulping and papermaking processes or the red liquid (acid system papermaking wastewater) that gives up, the molecular weight of this class industrial lignin, with plant material, pulp preparing process and condition are different bigger difference arranged, general wood type is than careless class height, and acid system is than alkaline process height.China's paper industry is based on alkaline process, and the annual industrial lignin that produces from pulping and paper-making surpasses 6,000,000 tons, and except that the alkali recovery was done in some burnings, major part was not utilized at present, becomes a big obstacle of contaminate environment restriction paper industry development.Industrial lignin is the profuse organic raw material resource in a kind of source, it has a lot of purposes, for example make tackiness agent, dispersion agent, tensio-active agent hangs down molecular product etc. with being degraded to, but directly utilizes its product performance of industrial lignin all undesirable, one of reason is the requirement that its molecular weight size can not adapt to product, for example make wood adhesive because the industrial lignin molecular weight is higher, and the tackiness agent of making can not be deep into timber inside, thereby its performance is total not as good as synthetic macromolecule glue; And for example make dispersion agent requirement high-molecular weight xylogen,, need improve its molecular weight by the chemical reaction method of complexity because existing industrial lignin can not meet the demands; Require molecular weight moderate when and for example industrial lignin is made the raw material of synthetic surfactant, existing industrial lignin molecular weight is higher, need to reduce its molecular weight with chemical process or thermochemical method, but because lignin molecule is a tridimensional network, C-C is not easy fracture, and it is all comparatively difficult to reduce its molecular weight with chemical process or thermochemical method.
Electrochemical method provided by the invention carries out electrochemical polymerization and degraded to industrial lignin, improves molecular weight and reduces the molecular weight purpose to reach.
Method of the present invention is that industrial lignin solution is placed in the reactor, inserts anode and negative electrode in this reactor.Used cathode material is plumbous, iron, stainless steel, nickel, carbon etc.; Anode material is to use platinum, gold, or on titanium base or non-metallic material, plate plumbic oxide.Industrial lignin solution both can be the aqueous solution, also can be non-aqueous solution, for sulfonated lignin and alkali lignin water as solvent commonly used.Solution pH value 2～13 when carrying out electrochemical reaction, 15～45 ℃ of temperature add 2～13 volts of volts DSs, 1～90 hour reaction times.Xylogen provided by the present invention had both contained certain material of xylogen, as timber, industrial lignin that non-wood timber matter fiber also can be separated from timber or non-wood timber matter fiber such as alkaline process xylogen, acid system xylogen, solvent xylogen, enzyme process xylogen etc.
Chemistry is compared with degradation method with the thermochemistry polymerization in the xylogen that electrochemical method provided by the invention is made different molecular weight and the prior art, has following advantage:
1. can be without other expensive catalysts and chemical reagent;
2. xylogen does not need strict the separation, and this method has higher selectivity and specificity;
3. reaction conditions relaxes, and does not need high temperature, high pressure;
4. reaction is nuisanceless, cleaning activity.
Use the xylogen of method preparation provided by the present invention and can make the dye well cement dispersants, when making cement dispersants, can significantly improve the flowability of cement; Can be used as the raw material of synthetic surfactant, the synthetic tensio-active agent, being used for tertiary oil recovery has low interfacial tension; Can be used as the starting material of synthetic macromolecule.
Embodiment 1:
Molecular weight is 3700 sodium lignosulfonate, 20 grams, and distilled water 156 grams are made into pH value and are 10 solution, and the electrode of putting into titanium aperture plate plating plumbic oxide is that anode, stainless (steel) wire are the reactor of negative electrode, adds 4 volts of volts DSs, reacts 10 hours down at 30 ℃.Obtain molecular weight and be the product of 5400 sodium lignosulfonate, this product has good dispersing property to cement, mixes 0.5% this product in cement, and the cement flows degree is 245mm, and correlated sample is 170mm.
Embodiment 2:
Molecular weight is 2400 alkali lignin 18 grams, distilled water 188 grams, be made into pH value and be 12 solution, inject in example 1 reactor, add 6 volts of volts DSs, under 30 ℃, reacted 38 hours, the acquisition molecular weight is 820 product, and with this product synthetic lignin surfactant 0.8% concentration, its oil water interfacial tension is 7 * 10 in composite displacement system
-3MN/m, and correlated sample is 8 * 10
-2MN/m.This tensio-active agent can be used in the tertiary oil recovery.
Embodiment 3:
Molecular weight is 4200 calcium lignin sulphonate 15 grams, distilled water 200 gram, being made into pH value with NaOH is 11.5 solution, the electrode of putting into cellular plastic net plating plumbic oxide is that anode, stainless (steel) wire are the reactor of negative electrode, add 5 volts of volts DSs, reacted 25 hours down at 25 ℃.The acquisition molecular weight is 1400 lignosulfonic acid calcium product, and 50% phenolic compound with in this product replacement resol obtains the resol identical performance synthetic with 100% phenolic compound.
Claims (2)
1, a kind of method of using the xylogen of electrochemical production different molecular weight, it is characterized in that be anode at device with titanium aperture plate plating plumbic oxide, stainless (steel) wire is in the chemical reactor of negative electrode, 4 volts of voltages, 30 ℃ of temperature, pH value of solution value 10,10 hours reaction times, under DC electric field, sulfonated lignin carry out polymerization, and xylogen is degraded.
2,, it is characterized in that described anode is a cellular plastic net plating plumbic oxide according to the method for the xylogen of the usefulness electrochemical production different molecular weight described in the claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001310011A CN1151195C (en) | 2000-12-27 | 2000-12-27 | Electrochemical process of preparing lignin in different molecular weight |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001310011A CN1151195C (en) | 2000-12-27 | 2000-12-27 | Electrochemical process of preparing lignin in different molecular weight |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1361193A CN1361193A (en) | 2002-07-31 |
| CN1151195C true CN1151195C (en) | 2004-05-26 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB001310011A Expired - Fee Related CN1151195C (en) | 2000-12-27 | 2000-12-27 | Electrochemical process of preparing lignin in different molecular weight |
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| CN (1) | CN1151195C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102277591B (en) * | 2011-08-02 | 2014-03-05 | 北京化工大学 | Method for electrochemically degrading lignin |
| CN103074639B (en) * | 2013-02-04 | 2015-04-29 | 河北工业大学 | Method for preparing 2, 6-ditertiary butyl-4-methylphenol by electrochemically degrading lignin |
| CN106987862B (en) * | 2017-04-12 | 2018-03-09 | 中北大学 | A kind of method of the electrochemical degradation lignin in eutectic solvent |
| CN108823595B (en) * | 2018-07-12 | 2020-05-01 | 东北石油大学 | Method for electrolyzing lignin at high temperature in solar STEP process |
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2000
- 2000-12-27 CN CNB001310011A patent/CN1151195C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1361193A (en) | 2002-07-31 |
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