CN1174030C - Method for producing sulfonated lignin - Google Patents
Method for producing sulfonated lignin Download PDFInfo
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- CN1174030C CN1174030C CNB021008051A CN02100805A CN1174030C CN 1174030 C CN1174030 C CN 1174030C CN B021008051 A CNB021008051 A CN B021008051A CN 02100805 A CN02100805 A CN 02100805A CN 1174030 C CN1174030 C CN 1174030C
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- black liquor
- sulfonated lignin
- sulphite
- reaction
- producing sulfonated
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Abstract
The present invention relates to a method for preparing lignosulphonate from black liquor of grass pulp paper making at a normal temperature at normal pressure. The present invention provides a method for generating lignosulphonate by sulphonating black liquor of pulping with an alkaline method at the normal temperature at the normal pressure for the problem of strict requirements for reaction conditions of a common sulphonation reaction needing to be carried out at a high temperature at high pressure. The method comprises the following steps: the black liquor coming from the primary pulp in a spherical boiler is extracted; the black liquor is supplied into an evaporator and concentrated by evaporation; a sulphonation reaction is carried out at the normal temperature at the normal pressure, formaldehyde is firstly added, and sulphite is secondly added and heated to react; the reaction product is supplied into a drying tower, dried and made into powder. Due to the addition of the formaldehyde and the sulphite in the sulphonation reaction, the sulphonation reaction can be carried out at the normal temperature at the normal pressure. The product containing a plurality of active groups, such as sulphonic groups, carboxy groups, etc., has the advantages of good solubility performance, high surface activity and superior dispersion performance. The product is mainly used for dispersing and filling dispersed dyes, reduced dyes and coal water slurry.
Description
Technical field
The present invention relates to a kind of method of producing sulfonated lignin, especially a kind of method of producing sulfonated lignin at normal temperature and pressure by the black liquor of papermaking straw pulp.
Background technology
The processing of alkaline pulping black liquor, the one, Silvola recovery, the 2nd, be dried to the powder method, produce alkali lignin.Silvola recovery exists investment big, cost height, working cost height, problem such as sewage disposal is not thorough.Be dried to the alkali lignin that powder generates, not only cheap, and the selling market is single.In chemical industry, general sulfonation reaction is carried out under High Temperature High Pressure, and its reaction conditions requires than higher, and reaction vessel must can bear certain reaction pressure, and general internal pressure pot pressure is 2.5kg/cm
2, outer pot pressure is 6.0kg/cm
2, could guarantee to react and normally carry out.
Summary of the invention
The objective of the invention is at the problems referred to above, a kind of black liquor sulfonation at normal temperatures and pressures with alkaline process is provided, generate the method for sulfonated lignin.
The method of producing sulfonated lignin of the present invention comprises the steps:
1. extract from the black liquor in the rotary spherical digester magma;
2. described black liquor is sent into evaporation concentration in the vaporizer, make its concentration reach 32～37%;
3. carry out sulfonation reaction at normal temperatures and pressures, add the formaldehyde that accounts for black liquor solid weight 4～6%, be heated to 55～65 ℃, reacted 80～100 minutes.
4. add the sulphite that accounts for black liquor solid weight 14～16% then, be heated to 95～100 ℃, reacted 80～100 minutes;
5. send into and carry out spraying drying in the drying tower, make moisture≤5%, make powder.
The method of producing sulfonated lignin of the present invention, wherein the sulphite that adds in four steps is S-WAT or calcium sulfite.
The method of producing sulfonated lignin of the present invention, wherein magma described in the first step is extracted black liquor through three extrusion equipments.
The method of producing sulfonated lignin of the present invention, wherein the vaporizer in second step is the limbs triple-effect evaporator.
Advantage of the present invention and positively effect are because sulfonation reaction adds formaldehyde and sulphite, can carry out sulfonation reaction at normal temperatures and pressures, the sodium lignosulfonate in market is compared with the wood lignin sodium sulfonate, this product contains more sulfonic group and carboxyl isoreactivity gene, have solubility property and higher surface activity and dispersing property preferably, be mainly used in the dispersion and the filling of dispersed dye and vat dyes and coal water slurry.It is good to have grinding-aid effect, advantage such as surfactivity, dispersiveness, thermostability, high dispersion stability are good.
Other details of the present invention and characteristics can be cheer and bright by reading the embodiment hereinafter encyclopaedize.
Embodiment
Be example to produce sodium lignosulfonate below, the production method of normal temperature and pressure of the present invention is described, comprise the steps:
1. extract black liquor from the magma of rotary spherical digester through three extrusion equipments.
2. described black liquor is sent into evaporation concentration in the limbs triple-effect evaporator; Make its concentration reach 32～37%, be preferably 35%;
3. carry out sulfonation reaction at normal temperatures and pressures, at first add formaldehyde, the amount that wherein adds formaldehyde accounts for 4～6% of black liquor solid weight, is preferably 5%, heats 55～65 ℃, reacts 80～100 minutes;
4. add S-WAT or calcium sulfite then, the amount that wherein adds S-WAT or calcium sulfite accounts for 14～16% of black liquor solid weight, is preferably 15%, heats 95～100 ℃, reacts 80～100 minutes.
5. send into and carry out spraying drying in the drying tower, make moisture≤5% wherein, make powder.
The sodium lignosulfonate that the method for the invention is made is a chocolate brown powder, pH value is 7-8, can transfer to 9-11 or 5-6 according to user's needs, water-insoluble≤0.2%, reduzate content≤4%, dispersion force 〉=100, heat-resistant stability is 130 ℃ of 4-5, moisture≤2%, fineness are 80 order percent of pass 〉=95%.Its main application is: slurries additive agent; Asphalt emulsifier; The printing and dyeing promoting agent; The tertiary oil production in oil field glidant; Concrete admixture; The pesticide producing dispersion agent; Refractory materials, ceramic disperse bonding, water-reducing strengthening agent; Production of phosphate fertilizer, ore pulp water reducer; Long-acting slowly released nitrogen fertilizer agent, the agent of high-efficiency sustained-release composite fertilizer; Sand prevention, sand-fixation agent etc.
Claims (6)
1. the method for a producing sulfonated lignin is characterized in that comprising the steps:
1. extract from the black liquor in the rotary spherical digester magma;
2. described black liquor is sent into evaporation concentration in the vaporizer, make its concentration reach 32～37%;
3. carry out sulfonation reaction at normal temperatures and pressures, add the formaldehyde that accounts for black liquor solid weight 4～6%, be heated to 55～65 ℃, reacted 80～100 minutes;
4. add the sulphite that accounts for black liquor solid weight 14～16% then, be heated to 95～100 ℃, reacted 80～100 minutes;
5. send into and carry out spraying drying in the drying tower, make moisture≤5%, make powder.
2. the method for producing sulfonated lignin according to claim 1 is characterized in that the amount that adds formaldehyde accounts for 5% of black liquor solid weight.
3. the method for producing sulfonated lignin according to claim 2 is characterized in that the amount that adds sulphite accounts for 15% of black liquor solid weight.
4. according to the method for the described producing sulfonated lignin of claim 1,2 or 3, it is characterized in that the sulphite that adds is S-WAT or calcium sulfite.
5. the method for producing sulfonated lignin according to claim 4 is characterized in that magma described in the first step is through three extrusion equipments extraction black liquor.
6. the method for producing sulfonated lignin according to claim 5 is characterized in that the vaporizer in second step is the limbs triple-effect evaporator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021008051A CN1174030C (en) | 2002-01-24 | 2002-01-24 | Method for producing sulfonated lignin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021008051A CN1174030C (en) | 2002-01-24 | 2002-01-24 | Method for producing sulfonated lignin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1434068A CN1434068A (en) | 2003-08-06 |
| CN1174030C true CN1174030C (en) | 2004-11-03 |
Family
ID=27627280
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021008051A Expired - Fee Related CN1174030C (en) | 2002-01-24 | 2002-01-24 | Method for producing sulfonated lignin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1174030C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009030122A1 (en) * | 2007-08-22 | 2009-03-12 | Guozhong Chen | A method for producing concrete water reducer by grafting of lignosulfonate with carbonyl group aliphatics |
| US10227666B2 (en) * | 2015-12-10 | 2019-03-12 | Industrial Technology Research Institute | Solid catalysts and method for preparing sugars using the same |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102078780B (en) * | 2011-01-11 | 2014-08-06 | 福州大学 | Modified lignin vat dye dispersing agent and preparation process thereof |
| CN102140174B (en) * | 2011-03-08 | 2014-01-29 | 延边石岘白麓纸业股份有限公司 | Preparation method for lignosulfonate |
| CN102251433A (en) * | 2011-07-06 | 2011-11-23 | 延边石岘白麓纸业股份有限公司 | Method for preparing paper |
| CN103819687B (en) * | 2014-03-21 | 2016-02-03 | 河南省科学院化学研究所有限公司 | A kind of method utilizing high sulphur coal to produce sodium lignosulfonate |
| CN104892956B (en) * | 2015-06-24 | 2017-12-29 | 济南圣泉集团股份有限公司 | Modified lignin mahogany sulfonate and preparation method thereof |
| CN104892954B (en) * | 2015-06-24 | 2017-12-05 | 济南圣泉集团股份有限公司 | Modified lignin mahogany sulfonate and preparation method thereof |
| CN104961899A (en) * | 2015-06-24 | 2015-10-07 | 济南圣泉集团股份有限公司 | Dye dispersant and preparation method thereof |
-
2002
- 2002-01-24 CN CNB021008051A patent/CN1174030C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009030122A1 (en) * | 2007-08-22 | 2009-03-12 | Guozhong Chen | A method for producing concrete water reducer by grafting of lignosulfonate with carbonyl group aliphatics |
| US10227666B2 (en) * | 2015-12-10 | 2019-03-12 | Industrial Technology Research Institute | Solid catalysts and method for preparing sugars using the same |
| US10883151B2 (en) * | 2015-12-10 | 2021-01-05 | Industrial Technology Research Institute | Solid catalysts |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1434068A (en) | 2003-08-06 |
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