CN1004891B - Method for mfg. dissolvable lignin from alkali lignin - Google Patents
Method for mfg. dissolvable lignin from alkali lignin Download PDFInfo
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- CN1004891B CN1004891B CN86107289.8A CN86107289A CN1004891B CN 1004891 B CN1004891 B CN 1004891B CN 86107289 A CN86107289 A CN 86107289A CN 1004891 B CN1004891 B CN 1004891B
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- lignin
- acetone
- alkali
- alkali lignin
- alcohol
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Abstract
The present invention relates to a method. In the method, alkali lignin is added in an organic solution to be processed in a pressure reactor at a certain temperature for certain periods to be converted into lignin which can be dissolved in an ordinary organic solvent; the organic solvent in which the obtained lignin is added can be methyl alcohol, ethyl alcohol, acetone, a mixture of the methyl alcohol, the ethyl alcohol and acetone, or a water solution of the methyl alcohol, the ethyl alcohol or the acetone; the processing temperature is from 170 DEG C to 210 DEG C, and the time is from 5 to 120 minutes. The obtained dissolvable lignin can be dissolved in acetone, methyl ethyl ketone, a mixture of acetone and alcohol, and ethanol or propyl alcohol heated above 50 DEG C, can be directly used as products or can be used as raw material for further chemical processing.
Description
The invention belongs to chemical treatment to plant lignin.
For the processing of black liquor of pulp making that with the vegetable fibre is alkaline process (sodium hydroxide method or the sulphate process) paper mill of raw material, external traditional method is that black liquor is concentrated afterfire, reclaim heat and alkali, at present, the black liquor of pulp making burning of China many alkaline processes factory is had any problem, and does not find appropriate treatment process again, even the alkali lignin that extracts does not have excellent usage yet, thereby a large amount of black liquor directly have to be entered rivers and lakes, cause serious public hazards.It is the important channel of handling black paper-making liquid of alkali pulping that economy properly fully utilizes alkali lignin.
The alkali lignin of solid state is not dissolved in common cheap organic solvent, only can dissolve alkali lignin with price costlinesses such as dimethyl formamide, methyl-sulphoxide, deleterious solvent now, but because the cost height, can only be for the usefulness of scientific research, and do not have a practical value industrial.Thereby usually people can only be with the aqueous solution of alkali as solvent, but because the existence of alkali and water hinders even can't carry out the further chemical modification reaction of alkali lignin, the alkaline solution of this alkali lignin does not have direct purposes.Make the method for the lignin that is dissolved in common volatile organic solvent from the alkali lignin of the black liquor of pulp making in alkaline process paper mill precipitation gained, do not see any report at present both at home and abroad as yet, search the also discovery record relevant of database of " world patent " (1963～now), " United States Patent (USP) " (nineteen fifty～now) and " chemical abstracts " (1967～now) through online information retrieval with this problem.
The objective of the invention is to obtain a kind of method that makes alkali lignin be transformed into solvable lignin.Thereby a large amount of black liquor of comprehensive utilization alkaline process paper plant.The solvable lignin that make the black liquor had no economic worth originally become to be rich in purposes, demand is bigger, and solve problem of environmental pollution.Said solvable lignin is meant the lignin that can be dissolved in cheap common organic solvent (for example: acetone, butanone, acetone and alcoholic acid mixture or be heated to ethanol, propyl alcohol more than 50 ℃).
Solvable lignin can directly be made product and use, for example: be used for the lignify again of paper or as the toughener of paper; Also can be used as the raw material of further chemical process.When solvable lignin is dissolved in when carrying out chemical reaction in above-mentioned any organic solvent because its content of phenolic hydroxyl groups is bigger than original alkali lignin, and reactivity worth is good, therefore be more suitable in reaction that needs acidic conditions or the main reaction relevant with phenolic hydroxyl group.
Content of the present invention:
The solid state alkali lignin is put into the pressurized vessel that has the stirring or do not have stirring, add methyl alcohol, ethanol, propyl alcohol, acetone or the mixture of these organic solvents and their aqueous solution.The solid-to-liquid ratio that adds is 1: 0.5～10, kept 5～120 minutes down for 170 ℃～210 ℃ in temperature, alkali lignin can be transformed into solvable lignin.
Optimal conditions are to be 50%～60% aqueous ethanolic solution with concentration in the aforesaid method: solid-to-liquid ratio is 1: 1～3; 180 ℃～200 ℃ of temperature, 15～30 minutes time.
Advantage of the present invention is that technological process is simple, and the reaction times is short, and used ordinary organic solvents is cheap and nontoxic, does not produce secondary pollution, for solution pollutes the handling problem of the alkaline pulping black liquor of environment, provides an effective way.
The contriver once had following embodiment:
At first pouring 10 gram alkali lignins into 20 gram concentration is to mix in 50% aqueous ethanolic solution or the aqueous acetone solution, then mixture is poured into ability 30 kilograms per centimeter
2In the pressurized vessel of pressure, put into 190 ℃ of constant temperature oil baths heating 15 minutes after the sealing, take out and be cooled to room temperature, open container, after pouring out or not pouring out supernatant liquid, add acetone solvable lignin is dissolved into solution.In heat-treatment process, alkali lignin becomes even single-phase existence with ethanolic soln, cooling back layering, and most of ethanolic soln (being dissolved with the part lignin) is separated in the upper strata, and the lignin of swollen is in lower floor.If take advantage of the hot type material, can become even single-phase discharge.As the solvable lignin that the need manufacturing is done, can evaporate to remove and desolvate and moisture.
Claims (4)
1, a kind of method that makes solvable lignin with alkali lignin, it is characterized in that the alkali lignin that it extracts with alkaline pulping black liquor is a raw material, add following any one organic solvent: methyl alcohol, ethanol, propyl alcohol, acetone or the mixture between them, and their aqueous solution, and the solid-to-liquid ratio that makes alkali lignin and organic solvent is 1: 0.5～10, place the pressure vessel sealing to heat to 170 ℃～210 ℃ then, the hold-time is 5～120 minutes.
2, according to claim 1ly a kind ofly make the method for solvable lignin, it is characterized in that adding concentration and be 50%～60% aqueous ethanolic solution with alkali lignin.
3, according to claim 1ly a kind ofly make the method for solvable lignin with alkali lignin, the solid-to-liquid ratio that it is characterized in that alkali lignin and organic solvent is 1: 1～3.
4, according to claim 1ly a kind ofly make the method for solvable lignin with alkali lignin, it is characterized in that sealing is heated to 180 ℃～200 ℃ in the pressure vessel, the hold-time is 15～30 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86107289.8A CN1004891B (en) | 1986-10-23 | 1986-10-23 | Method for mfg. dissolvable lignin from alkali lignin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86107289.8A CN1004891B (en) | 1986-10-23 | 1986-10-23 | Method for mfg. dissolvable lignin from alkali lignin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN86107289A CN86107289A (en) | 1988-05-04 |
| CN1004891B true CN1004891B (en) | 1989-07-26 |
Family
ID=4803551
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN86107289.8A Expired CN1004891B (en) | 1986-10-23 | 1986-10-23 | Method for mfg. dissolvable lignin from alkali lignin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1004891B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102503990B (en) * | 2011-09-22 | 2014-07-30 | 华南理工大学 | Method for preparing surfactant by taking lignin thermo-chemically degraded phenol product as raw material |
| CN108456312B (en) * | 2018-01-31 | 2021-01-29 | 齐鲁工业大学 | Method for preparing nano lignin by taking alkali lignin or sulphate lignin as raw material |
| CN110218336A (en) * | 2019-06-26 | 2019-09-10 | 南京工业大学 | Method for obtaining lignin with high phenolic hydroxyl content from residue after degradation and conversion of hemicellulose |
-
1986
- 1986-10-23 CN CN86107289.8A patent/CN1004891B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN86107289A (en) | 1988-05-04 |
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