Lignin materials containing compositions

Abstract

The present invention primarily relates to a preparation comprising or consisting of 40-99.9 wt.-% of lignin, preferably unmodified lignin, 0.1-50 wt.-% of minerals, preferably 0.1-30 wt.-%, 0-25 wt.-% of one or more mono- and oligomeric carbohydrates, preferably 0.1-20 wt.-%, and 0-15 wt.-% of one or more solvents, in particular water, preferably 0.1-4 wt.-%. Furthermore, the present invention relates to a fertilizer comprising or consisting of such a preparation and to the use of such a preparation as fertilizer, as ingredient for a fertilizer or for producing a fertilizer.

Claims

1. A preparation comprising: 60-99 wt.-% of unmodified lignin, and 1-20 wt.-% of minerals, and further comprising: 0.1-2 wt.-% of one or more mono- and oligomeric carbohydrates, and/or 0.1-2 wt.-% of one or more solvents; wherein the preparation is essentially free of cellulose and hemicellulose.

2. The preparation according to claim 1, wherein the preparation further comprises one or more components selected from the group consisting of hydrolysation products of cellulose and/or hemicellulose.

3. The preparation according to claim 1, wherein the preparation comprises a total carbohydrate content of less than 3 wt.-%.

4. The preparation according to claim 1 wherein one, more than one, or all of the minerals is/are selected from the group consisting of salts comprising K.sup.t, Na.sup.+, Ca.sup.2+, Mg.sup.2+, Cl.sup., PO.sub.4.sup.3 and SO.sub.4.sup.2.

5. The preparation according to claim 1, wherein the content of N is in the range of 0.1-15 wt.-%, and/or S is in the range of 0.1-5 wt.-%, based on the total weight of the preparation.

6. A preparation according to claim 1, wherein the preparation is obtained by a method for isolating lignin from a mixture comprising lignin, a cellulose solvent, a cellulose precipitant, minerals, and optionally cellulose and/or hemicellulose and/or hydrolysation products thereof, comprising the following steps: i) removing the cellulose precipitant from the mixture, ii) contacting the mixture with a lignin precipitant to obtain a precipitate, iii) removing the precipitate obtained in step ii) from the mixture, iv) optionally washing the precipitate with a lignin precipitant, v) removing the lignin precipitant from the precipitate, vi) optionally separating the cellulose solvent and the lignin precipitant from the remaining mixture obtained in step iii) with the proviso that in case the cellulose precipitant is the same as the lignin precipitant used in step ii) or contains one or more components of the mixture used as lignin precipitant in step ii), step i) is optional only.

7. Fertilizer comprising a preparation according to claim 1.

8. The preparation according to claim 1 comprising: 0.1-2 wt.-% of one or more solvents.

9. A preparation according to claim 1 comprising: 70-99 wt.-% of lignin, 1-10 wt.-% of minerals, 0.1-2 wt.-% of mono. and oligomeric carbohydrates, and 0.1-0.5 wt.-% of one or more solvents.

10. The preparation according to claim 1, wherein the preparation comprises xylose.

11. The preparation according to claim 1, wherein the content of N is in the range of 0.1-5 wt.-%, and/or S is in the range of 0.1-3 wt.-%, based on the total weight of the preparation.

12. The preparation according to claim 1, wherein the content of N is in the range of 0.1-3 wt.-%, and/or S is in the range of 0.1-1 wt.-%, based on the total weight of the preparation.

13. The preparation according to claim 1, wherein the one or more solvents comprise water.

14. The preparation according to claim 9, wherein the one or more solvents comprise water.

15. A preparation according to claim 5 comprising xylose.

16. A preparation according to claim 9 comprising xylose.

17. Fertilizer comprising a preparation according to claim 9.

Description

Example 1: Method for Digesting Lignocelluloses Containing Biomass Using a Cellulose Solvent and a Cellulose Precipitant (To Obtain a Pulping Slurry)

(1) Lignocellulose containing biomass in the form of 50 g of coarsely grained wheat straw was stirred with 300 ml 80% H.sub.3PO.sub.4 as cellulose solvent at 55 C. for 45 min to the complete solution of the straw. The black viscous medium was cooled to approx. 40 C. and then mixed vigorously with 600 ml of pre-cold MtB ether (methyl-tert. butylether) as a precipitant to give a compact precipitate of cellulose/hemicellulose. The solid phase was removed from the slurry.

Example 2: Method for Digesting Lignocelluloses Containing Biomass Using a Cellulose Solvent and a Cellulose Precipitant in Combination with a Lignin Solvent (To Obtain a Pulping Slurry)

(2) Lignocellulose containing biomass in the form of 30 g solid biogas digestate were mixed with 200 ml 80% H.sub.3PO.sub.4 as cellulose solvent and stirred at 50 C. for 40 min. The solution is precipitated with 1 l pre-cold mixture of ethanol/acetone as precipitant with a ratio of 3:1. The solid phase (the precipitate) was separated by centrifugation and the supernatant was collected.

Example 3: Method to Obtain a Preparation According to the Invention From a Pulping Slurry Obtained According to Example 1

(3) i) The organic cellulose precipitant was removed under reduced pressure of 400 mbar from the collected supernatant of example 1 to give a black viscous solution, which was cooled to 40 C.

(4) ii) 10 ml of the black solution was mixed vigorously with 50 ml ethyl acetate, which readily formed a brown precipitate.

(5) iii) The brown precipitate was filtered of. The filtrate was collected for later treatment.

(6) iv) The solids were suspended in another 50 ml ethyl acetate and filtered again. The filtrate was collected for later use in a step ii).

(7) v) The brown solids were dried at 65 C.

(8) vi) The ethyl acetate was removed from the phosphoric acid by distillation leaving approx. 8 ml.

(9) The regenerated acid of step vi) was able to dissolve 1.5 g of straw.

(10) The carbohydrate and ash content of the solids of step v) were determined as well as the element composition of to confirm that the brown precipitate was lignin.

(11) TABLE-US-00001 Parameter % of dry weight Sample weight 217 mg Ash 5% Carbohydrate 0.9% Lignin 90% Elementary analysis: C 64.8% H 4.5% O 28.8% N 0.8% S 0.4%

Example 4: Method to Obtain a Preparation According to the Invention From a Pulping Slurry Obtained According to Example 2

(12) i) The organic cellulose precipitant was removed under reduced pressure of 500 mbar from the collected supernatant of example 2 to give a black viscous solution, which was cooled to 40 C.

(13) ii) 20 ml of the black solution was mixed vigorously with 40 ml di-propyl ether, which readily formed a brown precipitate.

(14) iii) The brown precipitate was filtered of. The filtrate was collected for later treatment.

(15) iv) The solids were suspended in another 40 ml di-propyl ether and filtered again. The filtrate was collected for later use in a step ii). The brown solids were washed with 20 ml hot water.

(16) v) The brown solids were dried at 65 C.

(17) vi) The di-propyl ether was removed from the phosphoric acid by distillation leaving approx. 17 ml.

(18) The regenerated acid of step vi) was able to dissolve 2.5 g of straw.

(19) The carbohydrate and ash content of the solids of step v) were determined.

(20) TABLE-US-00002 Parameter % of dry weight Sample weight 750 mg Ash 18% Carbohydrate <0.1% Lignin 81% Elementary analysis: C 62.5% H 5% O 29% N 1% S 0.2%