CN113817177A - Modified lignosulfonate dispersant, preparation method and application in coal water slurry - Google Patents
Modified lignosulfonate dispersant, preparation method and application in coal water slurry Download PDFInfo
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- CN113817177A CN113817177A CN202110808309.3A CN202110808309A CN113817177A CN 113817177 A CN113817177 A CN 113817177A CN 202110808309 A CN202110808309 A CN 202110808309A CN 113817177 A CN113817177 A CN 113817177A
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- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G OR C10K; LIQUIFIED PETROLEUM GAS; USE OF ADDITIVES TO FUELS OR FIRES; FIRE-LIGHTERS
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- C10L1/32—Liquid carbonaceous fuels consisting of coal-oil suspensions or aqueous emulsions or oil emulsions
- C10L1/326—Coal-water suspensions
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Abstract
The invention relates to the technical field of modified lignin, a preparation method and application thereof, in particular to a modified lignosulfonate dispersant, a preparation method and application thereof in coal water slurry, wherein the modified lignosulfonate dispersant is obtained by the following method: dissolving sodium sulfite in water to obtain a solution 1; adding acetone into the solution 1 to react to obtain a solution 2; adding lignin into the solution 2, and carrying out constant-temperature reaction to obtain a solution 3; raising the reaction temperature of the solution 3, and adding formaldehyde in the heating process, wherein the formaldehyde is dropwise added when the temperature reaches 80-110 ℃; and then reacting at constant temperature to obtain the aliphatic modified lignosulfonate dispersant. The method adopts a grafting sulfonation mode to prepare the lignin dispersing agent with high molecular weight and high sulfonic acid group content, thereby improving the dispersibility of the lignin dispersing agent and having better dispersion viscosity reduction effect on the coal water slurry.
Description
Technical Field
The invention relates to the technical field of modified lignin, a preparation method and application thereof, in particular to a modified lignosulfonate dispersant, a preparation method and application thereof in coal water slurry; the modified lignosulfonate dispersant is an aliphatic modified lignosulfonate dispersant.
Background
Lignin is the most abundant aromatic polymer in nature and the only natural resource that can provide renewable aromatic compounds, and the content of lignin is second to cellulose in nature. The industrial kraft lignin accounts for a large proportion of the industrial lignin at present, and the application of the lignin is greatly limited by the characteristics of complex structure, low purity, low reaction activity, heterogeneity (wide relative molecular weight distribution) and the like. Compared with lignosulfonate, alkali lignin is poor in water solubility and easy to aggregate, has a small molecular weight and low chemical reaction activity, and greatly limits industrial application of the alkali lignin. The molecular weight and the sulfonic acid group content of the lignosulfonate are main factors influencing the dispersibility, the lignosulfonate component with a larger molecular weight has stronger dispersibility, and the adsorption and the dispersibility of the calcium lignosulfonate are improved by sulfonation modification, however, the synthesis of the lignosulfonate with a high molecular weight and a high sulfonic acid group content is difficult.
The current common solution is to improve the content of the sulfonic acid group of lignin by using a method of modifying with a micromolecular sulfonating agent, but the method has the following limitations: the increase in the content and molecular weight of the sulfonic acid group is limited by the number of active sites on the lignin and therefore the improvement is limited; therefore, a new method is needed to be found to further improve the lignin molecular weight and the content of the sulfonic acid group, and further improve the dispersibility and the pulping concentration of the lignin.
Disclosure of Invention
The invention provides a modified lignosulfonate dispersant, a preparation method and application thereof in coal water slurry, overcomes the defects of the prior art, and can effectively solve the problem that the prior art is difficult to synthesize a high-molecular-weight and high-sulfonate-content lignosulfonate dispersant.
One of the technical schemes of the invention is realized by the following measures: a modified lignosulfonate dispersant has the following chemical structural formula:
The following is a further optimization or/and improvement of one of the above-mentioned technical solutions of the invention:
the modified lignosulfonate dispersant is obtained by the following method: dissolving required amount of sodium sulfite at the temperature of 30-60 ℃ to obtain solution 1; adding acetone with required amount into the solution 1 to react at constant temperature to obtain a solution 2; adding required amount of lignin into the solution 2, heating to 60-80 ℃, and reacting at constant temperature to obtain a solution 3; adding formaldehyde with required amount into the solution 3, increasing the temperature of the solution 3 in the feeding process, controlling the temperature of the solution 3 in the formaldehyde adding process to be below 80-90 ℃, and after the formaldehyde is added, increasing the temperature to 80-110 ℃ and carrying out constant temperature reaction to obtain the modified lignosulfonate dispersant.
Further, the mass ratio of the lignin to the sodium sulfite is 100:96 to 100: 24.
Further, the mass ratio of the lignin to the acetone is 100: 124 to 100: 31.
Furthermore, the lignin is obtained by separating and purifying more than one of wheat straw sulfate pulp black liquor, bagasse sulfate pulping black liquor and coniferous wood sulfate pulping black liquor.
Further, the mass ratio of the formaldehyde to the acetone is 50: 100 to 200: 100.
Further, formaldehyde solution is adopted, and the mass percent of the formaldehyde solution is 37%.
Further, the temperature of the solution 1 is 30 ℃ to 60 ℃.
Further, the temperature of the solution 2 obtained by the reaction is 30 ℃ to 60 ℃, and the reaction time is 10min to 100 min.
Further, the reaction temperature of the solution 3 obtained by the reaction is 60 ℃ to 80 ℃, and the reaction time is 30min to 300 min.
Further, the reaction temperature of the modified lignosulfonate dispersant obtained by the reaction is 80-110 ℃, and the reaction time is 2-8 h. The second technical scheme of the invention is realized by the following measures: a preparation method of the modified lignosulfonate dispersant in the technical scheme comprises the following steps: : dissolving required amount of sodium sulfite at the temperature of 30-60 ℃ to obtain solution 1; adding acetone with required amount into the solution 1 to react at constant temperature to obtain a solution 2; adding required amount of lignin into the solution 2, heating to 60-80 ℃, and reacting at constant temperature to obtain a solution 3; adding formaldehyde with required amount into the solution 3, increasing the temperature of the solution 3 in the feeding process, controlling the temperature of the solution 3 in the formaldehyde adding process to be below 80-90 ℃, and after the formaldehyde is added, increasing the temperature to 80-110 ℃ and carrying out constant temperature reaction to obtain the modified lignosulfonate dispersant.
The third technical scheme of the invention is realized by the following measures: the application of the modified lignosulfonate dispersant in the coal water slurry is disclosed in one technical scheme.
The method adopts a grafting sulfonation mode to prepare the lignin dispersing agent (namely the aliphatic modified lignosulfonate dispersing agent) with high molecular weight and high sulfonic acid group content, thereby improving the dispersibility of the lignin dispersing agent and having better dispersion viscosity reduction effect on the coal water slurry.
Drawings
FIG. 1 is a graph comparing an infrared spectrum of an aliphatic modified lignosulfonate dispersant prepared in example 1 of the present invention with that of lignin.
In fig. 1, Lignin represents Lignin, and G represents an aliphatic modified lignosulfonate dispersant.
Detailed Description
The present invention is not limited by the following examples, and specific embodiments may be determined according to the technical solutions and practical situations of the present invention. The solution in the present invention is an aqueous solution of water as a solvent unless otherwise specified.
The modified lignosulfonate dispersant is prepared by the following preparation method: dissolving required amount of sodium sulfite at the temperature of 30-60 ℃ to obtain solution 1; adding acetone with required amount into the solution 1 to react at constant temperature to obtain a solution 2; adding required amount of lignin into the solution 2, heating to 60-80 ℃, and reacting at constant temperature to obtain a solution 3; adding formaldehyde with required amount into the solution 3, increasing the temperature of the solution 3 in the feeding process, controlling the temperature of the solution 3 in the formaldehyde adding process to be below 80-90 ℃, and after the formaldehyde is added, increasing the temperature to 80-110 ℃ and carrying out constant temperature reaction to obtain the aliphatic modified lignosulfonate dispersant.
The mass ratio of the lignin to the sodium sulfite is 100:96 to 100: 24.
The mass ratio of the lignin to the acetone is 100: 124 to 100: 31.
The mass ratio of the formaldehyde to the acetone is 50: 100 to 200: 100.
The formaldehyde adopts formaldehyde solution, and the mass percent of the formaldehyde solution is 37%.
The temperature of the solution 1 is 30 ℃ to 60 ℃.
The temperature of the solution 2 obtained by the reaction is 30-60 ℃, and the reaction time is 10-100 min.
The reaction temperature of the solution 3 obtained by the reaction is 60-80 ℃, and the reaction time is 30-300 min.
The reaction temperature of the aliphatic modified lignosulfonate dispersant obtained by the reaction is 80-110 ℃, and the reaction time is 2-8 h.
The lignin can be the lignin which is generally sold on the market at present, and can also be obtained by separating and purifying more than one of wheat straw sulfate pulp black liquor, bagasse sulfate pulping black liquor and coniferous wood sulfate pulping black liquor.
The chemical structural formula of the prepared aliphatic modified lignosulfonate dispersant is as follows:
The preparation method of the aliphatic modified lignosulfonate dispersant adopts a grafting sulfonation mode to prepare the high-molecular-weight and high-sulfonate-content lignin dispersant, so that the dispersibility of the lignin dispersant is improved.
The invention is further described below with reference to specific examples:
example 1:
the aliphatic modified lignosulfonate dispersant is prepared by the following preparation method:
(1) 9.6g of sodium sulfite were dissolved in a reaction flask equipped with a temperature-controlled electric heating device, an electric stirrer, a thermometer, a dropping funnel and a reflux condenser, the temperature of the solution during the dissolution being maintained at 30 ℃.
(2) After the solution was clarified, 12.4g of acetone was added and reacted at 30 ℃ for 10 min.
(3) Then 10g of lignin powder is added into the reactor; the temperature was raised to 60 ℃ and maintained for another 30 min.
(4)6.2g of formaldehyde are introduced into the reactor via a dropping funnel. During the addition, the temperature of the solution is automatically increased and should be controlled below 80 ℃. And (2) reducing the loss of acetone and low molecular weight intermediates by adopting a strong reflux condenser, increasing the temperature to 80 ℃ after adding a formaldehyde solution, and continuously reacting for 2 hours to obtain the aliphatic modified lignosulfonate dispersant (G-1 for short).
Comparison of infrared spectra of the aliphatic modified lignosulfonate dispersant prepared in example 1 and lignin is shown in fig. 1, and it can be seen from fig. 1 that the aliphatic modified lignosulfonate dispersant can be prepared by the preparation method of the present invention.
Example 2:
the aliphatic modified lignosulfonate dispersant is prepared by the following preparation method:
(1) 2.4g of sodium sulfite was dissolved in a reaction flask equipped with a temperature-controlled electric heating device, an electric stirrer, a thermometer, a dropping funnel and a reflux condenser. The temperature of the solution was maintained at 30 ℃ during the dissolution.
(2) After the solution was clarified, 3.1g of acetone was added and reacted at 30 ℃ for 100 min.
(3) Then 10g of lignin powder is added into the reactor; the temperature was raised to 60 ℃ and maintained for another 300 min.
(4)6.2g of formaldehyde are introduced into the reactor via a dropping funnel. During the addition, the temperature of the solution is automatically increased and should be controlled below 80 ℃. And (3) reducing the loss of acetone and low molecular weight intermediates by adopting a strong reflux condenser, increasing the temperature to 80 ℃ after adding a formaldehyde solution, and continuously reacting for 8 hours to obtain the aliphatic modified lignosulfonate dispersant (G-2 for short).
Example 3:
the aliphatic modified lignosulfonate dispersant is prepared by the following preparation method:
(1) 7g of sodium sulfite was dissolved in a reaction flask equipped with a temperature-controlled electric heating device, an electric stirrer, a thermometer, a dropping funnel and a reflux condenser. The temperature of the solution was maintained at 60 ℃ during the dissolution.
(2) After the solution is clarified, 10g of acetone is added and the reaction is carried out for 10min at 60 ℃.
(3) Then 10g of lignin powder is added into the reactor; the temperature was raised to 80 ℃ and maintained for another 30 min.
(4)6g of formaldehyde are introduced into the reactor via a dropping funnel. During the addition, the temperature of the solution is automatically increased and should be controlled below 90 ℃. And (3) reducing the loss of acetone and low molecular weight intermediates by adopting a strong reflux condenser, increasing the temperature to 110 ℃ after adding a formaldehyde solution, and continuously reacting for 2 hours to obtain the aliphatic modified lignosulfonate dispersant (G-3 for short).
Example 4:
the aliphatic modified lignosulfonate dispersant is prepared by the following preparation method:
(1) 5g of sodium sulfite was dissolved in a reaction flask equipped with a temperature-controlled electric heating device, an electric stirrer, a thermometer, a dropping funnel and a reflux condenser. The temperature of the solution was maintained at 60 ℃ during the dissolution.
(2) After the solution was clarified, 8g of acetone was added and reacted at 60 ℃ for 100 min.
(3) Then 10g of lignin powder is added into the reactor; the temperature was raised to 80 ℃ and maintained for another 300 min.
(4)8g of formaldehyde are introduced into the reactor via a dropping funnel. During the addition, the temperature of the solution is automatically increased and should be controlled below 90 ℃. And (3) reducing the loss of acetone and low molecular weight intermediates by adopting a strong reflux condenser, increasing the temperature to 110 ℃ after adding a formaldehyde solution, and continuously reacting for 8 hours to obtain the aliphatic modified lignosulfonate dispersant (G-4 for short).
Example 5:
the aliphatic modified lignosulfonate dispersant is prepared by the following preparation method:
(1) 3g of sodium sulfite was dissolved in a reaction flask equipped with a temperature-controlled electric heating device, an electric stirrer, a thermometer, a dropping funnel and a reflux condenser. The temperature of the solution was maintained at 40 ℃ during the dissolution.
(2) After the solution was clarified, 6g of acetone was added and reacted at 40 ℃ for 70 min.
(3) Then 10g of lignin powder is added into the reactor; the temperature was raised to 65 ℃ and maintained for another 200 min.
(4)8g of formaldehyde are introduced into the reactor via a dropping funnel. During the addition, the temperature of the solution is automatically increased and should be controlled below 85 ℃. And (3) reducing the loss of acetone and low molecular weight intermediates by adopting a strong reflux condenser, increasing the temperature to 90 ℃ after adding a formaldehyde solution, and continuously reacting for 6 hours to obtain the aliphatic modified lignosulfonate dispersant (G-5 for short).
Example 6:
the aliphatic modified lignosulfonate dispersant is prepared by the following preparation method:
(1) 4g of sodium sulfite was dissolved in a reaction flask equipped with a temperature-controlled electric heating device, an electric stirrer, a thermometer, a dropping funnel and a reflux condenser. The temperature of the solution was maintained at 50 ℃ during the dissolution.
(2) After the solution was clarified, 4g of acetone was added and reacted at 50 ℃ for 30 min.
(3) Then 10g of lignin powder is added into the reactor; the temperature was raised to 75 ℃ and maintained for another 100 min.
(4)7g of formaldehyde are introduced into the reactor via a dropping funnel. During the addition, the temperature of the solution is automatically increased and should be controlled below 85 ℃. And (3) reducing the loss of acetone and low molecular weight intermediates by adopting a strong reflux condenser, increasing the temperature to 100 ℃ after adding a formaldehyde solution, and continuously reacting for 3 hours to obtain the aliphatic modified lignosulfonate dispersant (G-6 for short).
Example 7: the G-6 prepared in the embodiment is used for preparing the coal water slurry, a laboratory dry method is adopted for pulping in a pulping experiment, the pulping concentration is preset, the mass of a coal sample, water and the G-6 additive is calculated, in the invention, the adding amount of the G-6 is 0.5 wt% of the mass of dry coal powder, the three are mixed and stirred for 10min by a JJ-1 type electric stirrer, a water coal slurry sample is prepared, and the coal water slurry without the dispersant is used as a blank control group. The properties of the coal water slurry are mainly examined, and the results are shown in table 1.
As can be seen from Table 1, compared with a blank control group, the viscosity of the coal water slurry added with G-6 is reduced, and the slurry concentration is high, which shows that the aliphatic modified lignosulfonate dispersant has a good dispersion viscosity-reducing effect on the coal water slurry.
The molecular weight and sulfonic acid group content of the G-6 waste heat prepared in example 6 were 25700Da and 2.48mmol/G, respectively, both of which were about 100% higher than those of sodium lignosulfonate.
The technical characteristics form an embodiment of the invention, which has strong adaptability and implementation effect, and unnecessary technical characteristics can be increased or decreased according to actual needs to meet the requirements of different situations.
TABLE 1
| Coal kind | Shenhua mixed coal | Shenhua coal mixture-blank | Artificial horse coal | Coal of artificial horse-blank |
| Concentration of finished pulp% | 63.64 | 59.37 | 59.37 | 56.26 |
| Viscosity mPas | 400 | 412.2 | 736.7 | 743.8 |
| Fluidity of the resin | B- | B+ | B+ | B+ |
| Stability for 24h | B+ | B+ | B+ | B+ |
Claims (10)
1. A modified lignosulfonate dispersant is characterized by having a chemical structural formula as follows:
2. The modified lignosulfonate dispersant according to claim 1, characterized in being obtainable by: dissolving required amount of sodium sulfite at the temperature of 30-60 ℃ to obtain solution 1; adding acetone with required amount into the solution 1 to react at constant temperature to obtain a solution 2; adding required amount of lignin into the solution 2, heating to 60-80 ℃, and reacting at constant temperature to obtain a solution 3; adding formaldehyde with required amount into the solution 3, increasing the temperature of the solution 3 in the feeding process, controlling the temperature of the solution 3 in the formaldehyde adding process to be below 80-90 ℃, and after the formaldehyde is added, increasing the temperature to 80-110 ℃ and carrying out constant temperature reaction to obtain the modified lignosulfonate dispersant.
3. The modified lignosulfonate dispersant of claim 1 or 2, characterized in that the mass ratio of the lignin to the sodium sulfite is 100:96 to 100: 24; or/and the mass ratio of the lignin to the acetone is 100: 124 to 100: 31; or/and the mass ratio of the formaldehyde to the acetone is 50: 100 to 200: 100.
4. The modified lignosulfonate dispersant of claim 1, 2 or 3, wherein the lignin is obtained by separating and purifying at least one of wheat straw sulfate pulp black liquor, bagasse sulfate pulping black liquor and softwood sulfate pulping black liquor.
5. The modified lignosulfonate dispersant of any one of claims 1 to 4, characterized in that formaldehyde is a formaldehyde solution, the mass percentage of the formaldehyde solution being 37%; or/and the temperature of the solution 1 is 30 ℃ to 60 ℃.
6. The modified lignosulfonate dispersant of any one of claims 1 to 5, characterized in that the temperature of the reaction-resulting solution 2 is 30 ℃ to 60 ℃ and the reaction time is 10min to 100 min.
7. The modified lignosulfonate dispersant of any one of claims 1 to 6, characterized in that the reaction temperature of the reaction-obtained solution 3 is 60 ℃ to 80 ℃ and the reaction time is 30min to 300 min.
8. The modified lignosulfonate dispersant of any one of claims 1 to 7, wherein the reaction temperature for obtaining the modified lignosulfonate dispersant by the reaction is 80 ℃ to 110 ℃ and the reaction time is 2h to 8 h.
9. A method for preparing a modified lignosulfonate dispersant according to claim 7, characterized by the following steps: dissolving required amount of sodium sulfite at the temperature of 30-60 ℃ to obtain solution 1; adding acetone with required amount into the solution 1 to react at constant temperature to obtain a solution 2; adding required amount of lignin into the solution 2, heating to 60-80 ℃, and reacting at constant temperature to obtain a solution 3; adding formaldehyde with required amount into the solution 3, increasing the temperature of the solution 3 in the feeding process, controlling the temperature of the solution 3 in the formaldehyde adding process to be below 80-90 ℃, and after the formaldehyde is added, increasing the temperature to 80-110 ℃ and carrying out constant temperature reaction to obtain the modified lignosulfonate dispersant.
10. Use of a modified lignosulfonate dispersant according to any one of claims 1 to 8 in a coal water slurry.
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Application publication date: 20211221 |