CN109384938A - The method and its application of sodium lignin sulfonate are prepared using black liquid - Google Patents
The method and its application of sodium lignin sulfonate are prepared using black liquid Download PDFInfo
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- CN109384938A CN109384938A CN201811282957.4A CN201811282957A CN109384938A CN 109384938 A CN109384938 A CN 109384938A CN 201811282957 A CN201811282957 A CN 201811282957A CN 109384938 A CN109384938 A CN 109384938A
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- black liquid
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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Abstract
The present invention discloses the method for preparing sodium lignin sulfonate using black liquid, including (1) prepares black liquid concentrate；(2) absolute dry mass of lignin in black liquid concentrate is obtained；(3) pH value of black liquid concentrate is adjusted to 8.5~12.5, polymerization inhibitor is added thereto, then by 50 DEG C~140 DEG C 0.5~3h of reaction of mixed liquor；(4) formaldehyde, sodium sulfite, sodium hydrogensulfite, sulfur dioxide are sequentially added into reaction solution, then 70 DEG C~105 DEG C are filtered to get lignin sulfonic acid sodium water solution is arrived for reaction 1~3 hour.Sodium lignin sulfonate obtained by the above method is as dye dispersant.The method and its application disclosed by the invention for preparing sodium lignin sulfonate using black liquid have the advantages that 1, reduce and pollute and simplify processing step, shorten the production cycle, improve production efficiency；2, managing thermal stability is high, good hydrophilic property；3, the generation of acid waste water is significantly reduced.
Description
Technical field
The invention belongs to papermaking black liquor wastewater process fields, and in particular to prepare sodium lignin sulfonate using black liquid
Method and its application.
Background technique
Dyestuff is the substance that fiber and other materials can be made to colour, it, which should have, is not easy to decolourize, change colour, and dye-uptake is high, dye
The features such as color is uniform.In order to make dyestuff be uniformly dispersed, often need to add a kind of auxiliary agent thereto --- dye dispersant, it
It is a kind of auxiliary agent that can be improved and improve solid or liquid material dispersion performance, the dissolubility of dyestuff can be promoted to improve printing and dyeing
Effect.Dye dispersant is to have a large capacity and a wide range in processing aid, develop faster a kind of additive.It has lipophilic and parent simultaneously
Aqueous two kinds of groups, therefore, common dispersing agent is all surfactant.
Currently, common surfactant is lignin sulfonate, but traditional lignin sulfonate for preparing
Method is high to lignin ingredient requirement, and whens raw materials for production can generate a large amount of acid waste waters, directly outer if not treatment of acidic wastewater
Row can cause serious pollution to water body, if treatment of acidic wastewater, and cost could be increased to enterprise.
Currently, also someone uses sulfite cellulose black liquor to prepare lignosulfonates, although black liquid can either be improved
Added value, also can be realized the improvement to waste liquid, avoid pollution of the waste liquid to environment.However, lignin sulfonate
Dye dispersant coloration with higher itself, has large effect to dyeing effect, heavier to the staining of cloth, and its is resistance to
Thermal stability is also poor.
Summary of the invention
Goal of the invention: the present invention has made improvements in view of the above-mentioned problems of the prior art, i.e., the invention discloses utilizations
Black liquid prepares the method and its application of sodium lignin sulfonate.
Technical solution: the method for preparing sodium lignin sulfonate using black liquid, comprising the following steps:
(1) black liquid concentrate is prepared；
(11) it is sieved to black liquid, removes water-insoluble particle and fibrous impurity:
(12) film process is carried out by ceramic-film tube to the black liquid after sieving again, remove the small organic matter of molecular weight and
Part water obtains black liquid concentrate, in which:
The average pore size of ceramic-film tube is 1~5 μm；
(2) the black liquid concentrate that the step of measuring 0.5~10 gram (12) obtains, is dried at 100~180 DEG C, evaporation
Fall the moisture in black liquid concentrate, obtains lignin in the black liquid concentrate that 0.5~10 gram of step (12) obtains
Absolute dry mass；
(3) pH value of black liquid concentrate is adjusted to 8.5~12.5, and polymerization inhibitor is then added thereto, obtains after mixing
To mixed liquor, mixed liquor is then obtained into reaction solution in 50 DEG C~140 DEG C 0.5~3h of reaction, in which:
The amount of the substance of added polymerization inhibitor and the absolute dry mass ratio of lignin are (0.2~2.0) mmol:1g；
(4) formaldehyde, sodium sulfite, sodium hydrogensulfite, sulfur dioxide are sequentially added in the reaction solution obtained to step (3),
Then it is filtered after being reacted 1~3 hour at 70 DEG C~105 DEG C, obtaining filtrate is lignin sulfonic acid sodium water solution, in which:
The amount of the substance for the formaldehyde being added and the absolute dry mass ratio of lignin are (1.0~3) mmol:1g；
The amount of the substance for the sodium sulfite being added and the absolute dry mass ratio of lignin are (0.3~3) mmol:1g；
The amount of the substance for the sodium hydrogensulfite being added and the absolute dry mass ratio of lignin are (0.3~3) mmol:1g；
The amount of the substance for the sulfur dioxide being added and the absolute dry mass ratio of lignin are (0.3~3) mmol:1g.
Further, the black liquid in step (11) is sulfite cellulose black liquor.
Further, the sieve being sieved in step (11) is 200 mesh~1000 mesh.
Further, pass through the pH value of addition sodium hydroxide or sulfuric acid adjusting black liquid concentrate to 8.5 in step (3)
~12.5.
Further, the polymerization inhibitor is one or more of epoxychloropropane, formic acid, acetic acid, sodium chloroacetate.
Further, the time-consuming that sodium sulfite is added in step (3) is 45 minutes~240 minutes.
Sodium lignin sulfonate obtained by the above method is as dye dispersant.
The utility model has the advantages that it is disclosed by the invention using black liquid prepare sodium lignin sulfonate method and its application have with
It is lower the utility model has the advantages that
1, it simplifies processing step while reducing pollution, shorten the production cycle, improving production efficiency；
2, sodium lignin sulfonate its thermal stability height obtained, good hydrophilic property；
3, the generation of the acid waste water when extracting lignin is significantly reduced.
Specific embodiment:
Detailed description of specific embodiments of the present invention below.
Specific embodiment 1
The method for preparing sodium lignin sulfonate using black liquid, comprising the following steps:
(1) black liquid concentrate is prepared；
(11) it is sieved to black liquid, removes water-insoluble particle and fibrous impurity:
(12) film process is carried out by ceramic-film tube to the black liquid after sieving again, remove the small organic matter of molecular weight and
Part water obtains black liquid concentrate, in which:
The average pore size of ceramic-film tube is 1 μm；
(2) the black liquid concentrate that the step of measuring 0.5 gram (12) obtains, dries at 100 DEG C, evaporates black liquid
Moisture in concentrate obtains the absolute dry mass of lignin in the black liquid concentrate that 0.5 gram of step (12) obtains；
(3) pH value of black liquid concentrate is adjusted to 8.5, and polymerization inhibitor is then added thereto, is mixed after mixing
Then mixed liquor is obtained reaction solution in 50 DEG C of DEG C of reaction 3h by liquid, in which:
The amount of the substance of added polymerization inhibitor and the absolute dry mass ratio of lignin are 0.2mmol:1g；
(4) formaldehyde, sodium sulfite, sodium hydrogensulfite, sulfur dioxide are sequentially added in the reaction solution obtained to step (3),
Then it is filtered after reacting for 3 hours at 70 DEG C, obtaining filtrate is lignin sulfonic acid sodium water solution, in which:
The amount of the substance for the formaldehyde being added and the absolute dry mass ratio of lignin are 1mmol:1g；
The amount of the substance for the sodium sulfite being added and the absolute dry mass ratio of lignin are 0.3mmol:1g；
The amount of the substance for the sodium hydrogensulfite being added and the absolute dry mass ratio of lignin are 0.3mmol:1g；
The amount of the substance for the sulfur dioxide being added and the absolute dry mass ratio of lignin are 0.3mmol:1g.
Further, the black liquid in step (11) is sulfite cellulose black liquor.
Further, the sieve being sieved in step (11) is 200 mesh.
Further, in step (3) by be added sodium hydroxide or sulfuric acid adjust the pH value of black liquid concentrate to
8.5。
Further, the polymerization inhibitor is epoxychloropropane.
Further, the time-consuming that sodium sulfite is added in step (3) is 45 minutes.
Sodium lignin sulfonate obtained by the above method is as dye dispersant.
The sodium lignin sulfonate and Disperse Blue-79 # filter cake that specific embodiment 1 is prepared according to solid content 0.7:1 ratio
Sand mill 2 hours, takes out 2 milliliters of ground slurry and is placed on glass plate, glass plate is put into 130 DEG C of baking oven 5 minutes,
After measurement, the high-temperature stability of sodium lignin sulfonate manufactured in the present embodiment is good, hydrophily is good.
Specific embodiment 2
The method for preparing sodium lignin sulfonate using black liquid, comprising the following steps:
(1) black liquid concentrate is prepared；
(11) it is sieved to black liquid, removes water-insoluble particle and fibrous impurity:
(12) film process is carried out by ceramic-film tube to the black liquid after sieving again, remove the small organic matter of molecular weight and
Part water obtains black liquid concentrate, in which:
The average pore size of ceramic-film tube is 5 μm；
(2) the black liquid concentrate that the step of measuring 10 grams (12) obtains, dries at 180 DEG C, evaporates black liquid
Moisture in concentrate obtains the absolute dry mass of lignin in the black liquid concentrate that 10 grams of steps (12) obtain；
(3) pH value of black liquid concentrate is adjusted to 12.5, and polymerization inhibitor is then added thereto, is mixed after mixing
Then mixed liquor is obtained reaction solution in 140 DEG C of reaction 0.5h by liquid, in which:
The amount of the substance of added polymerization inhibitor and the absolute dry mass ratio of lignin are 2mmol:1g；
(4) formaldehyde, sodium sulfite, sodium hydrogensulfite, sulfur dioxide are sequentially added in the reaction solution obtained to step (3),
Then it is filtered after being reacted 1 hour at 105 DEG C, obtaining filtrate is lignin sulfonic acid sodium water solution, in which:
The amount of the substance for the formaldehyde being added and the absolute dry mass ratio of lignin are 3mmol:1g；
The amount of the substance for the sodium sulfite being added and the absolute dry mass ratio of lignin are 3mmol:1g；
The amount of the substance for the sodium hydrogensulfite being added and the absolute dry mass ratio of lignin are 3mmol:1g；
The amount of the substance for the sulfur dioxide being added and the absolute dry mass ratio of lignin are 3mmol:1g.
Further, the black liquid in step (11) is sulfite cellulose black liquor.
Further, the sieve being sieved in step (11) is 1000 mesh.
Further, in step (3) by be added sodium hydroxide or sulfuric acid adjust the pH value of black liquid concentrate to
12.5。
Further, the polymerization inhibitor is formic acid.
Further, the time-consuming that sodium sulfite is added in step (3) is 240 minutes.
Sodium lignin sulfonate obtained by the above method is as dye dispersant.
The sodium lignin sulfonate and Disperse Blue-79 # filter cake that specific embodiment 2 is prepared according to solid content 0.7:1 ratio
Sand mill 3 hours, takes out 2 milliliters of ground slurry and is placed on glass plate, glass plate is put into 160 DEG C of baking oven 5 minutes,
After measurement, the high-temperature stability of sodium lignin sulfonate manufactured in the present embodiment is good, hydrophily is good.
Specific embodiment 3
The method for preparing sodium lignin sulfonate using black liquid, comprising the following steps:
(1) black liquid concentrate is prepared；
(11) it is sieved to black liquid, removes water-insoluble particle and fibrous impurity:
(12) film process is carried out by ceramic-film tube to the black liquid after sieving again, remove the small organic matter of molecular weight and
Part water obtains black liquid concentrate, in which:
3 μm of the average pore size of ceramic-film tube；
(2) the black liquid concentrate that the step of measuring 5 grams (12) obtains, dries at 140 DEG C, it is dense to evaporate black liquid
Moisture in contracting liquid obtains the absolute dry mass of lignin in the black liquid concentrate that 5 grams of steps (12) obtain；
(3) pH value of black liquid concentrate is adjusted to 10, and polymerization inhibitor is then added thereto, is mixed after mixing
Then mixed liquor is obtained reaction solution in 70 DEG C of reaction 2h by liquid, in which:
The amount of the substance of added polymerization inhibitor and the absolute dry mass ratio of lignin are 1mmol:1g；
(4) formaldehyde, sodium sulfite, sodium hydrogensulfite, sulfur dioxide are sequentially added in the reaction solution obtained to step (3),
Then it is filtered after being reacted 2 hours at 90 DEG C, obtaining filtrate is lignin sulfonic acid sodium water solution, in which:
The amount of the substance for the formaldehyde being added and the absolute dry mass ratio of lignin are 2mmol:1g；
The amount of the substance for the sodium sulfite being added and the absolute dry mass ratio of lignin are 2mmol:1g；
The amount of the substance for the sodium hydrogensulfite being added and the absolute dry mass ratio of lignin are 2mmol:1g；
The amount of the substance for the sulfur dioxide being added and the absolute dry mass ratio of lignin are 2mmol:1g.
Further, the black liquid in step (11) is sulfite cellulose black liquor.
Further, the sieve being sieved in step (11) is 400 mesh.
Further, pass through the pH value of addition sodium hydroxide or sulfuric acid adjusting black liquid concentrate to 10 in step (3).
Further, the polymerization inhibitor is acetic acid.
Further, the time-consuming that sodium sulfite is added in step (3) is 120 minutes.
Sodium lignin sulfonate obtained by the above method is as dye dispersant.
The sodium lignin sulfonate and Disperse Blue-79 # filter cake that embodiment 3 is prepared are ground according to the ratio sand of solid content 0.7:1
It 2.5 hours, takes out 2 milliliters of ground slurry and is placed on glass plate, glass plate is put into 150 DEG C of baking oven 5 minutes, survey
After fixed, the high-temperature stability of sodium lignin sulfonate manufactured in the present embodiment is good, hydrophily is good.
Specific embodiment 4~13
Roughly the same with specific embodiment 1, difference is only in that polymerization inhibitor difference, has as shown in the table:
Embodiments of the present invention are elaborated above.But present invention is not limited to the embodiments described above,
Technical field those of ordinary skill within the scope of knowledge, can also do without departing from the purpose of the present invention
Various change out.
Claims (7)
1. the method for preparing sodium lignin sulfonate using black liquid, which comprises the following steps:
(1) black liquid concentrate is prepared；
(11) it is sieved to black liquid, removes water-insoluble particle and fibrous impurity:
(12) film process is carried out by ceramic-film tube to the black liquid after sieving again, removes molecular weight small organic matter and part
Water obtains black liquid concentrate, in which:
The average pore size of ceramic-film tube is 1~5 μm；
(2) the black liquid concentrate that the step of measuring 0.5~10 gram (12) obtains, dries at 100~180 DEG C, evaporates and make
Moisture in paper Black Liquor Concentration liquid obtains the over dry of lignin in the black liquid concentrate that 0.5~10 gram of step (12) obtains
Quality；
(3) pH value of black liquid concentrate is adjusted to 8.5~12.5, and polymerization inhibitor is then added thereto, is mixed after mixing
Liquid is closed, mixed liquor is then obtained into reaction solution in 50 DEG C~140 DEG C 0.5~3h of reaction, in which:
The amount of the substance of added polymerization inhibitor and the absolute dry mass ratio of lignin are (0.2~2.0) mmol:1g；
(4) formaldehyde, sodium sulfite, sodium hydrogensulfite, sulfur dioxide are sequentially added in the reaction solution obtained to step (3), then
It is filtered after being reacted 1~3 hour at 70 DEG C~105 DEG C, obtaining filtrate is lignin sulfonic acid sodium water solution, in which:
The amount of the substance for the formaldehyde being added and the absolute dry mass ratio of lignin are (1.0~3) mmol:1g；
The amount of the substance for the sodium sulfite being added and the absolute dry mass ratio of lignin are (0.3~3) mmol:1g；
The amount of the substance for the sodium hydrogensulfite being added and the absolute dry mass ratio of lignin are (0.3~3) mmol:1g；
The amount of the substance for the sulfur dioxide being added and the absolute dry mass ratio of lignin are (0.3~3) mmol:1g.
2. the method according to claim 1 for preparing sodium lignin sulfonate using black liquid, which is characterized in that step
(11) black liquid in is sulfite cellulose black liquor.
3. the method according to claim 1 for preparing sodium lignin sulfonate using black liquid, which is characterized in that step
(11) sieve being sieved in is 200 mesh~1000 mesh.
4. the method according to claim 1 for preparing sodium lignin sulfonate using black liquid, which is characterized in that step
(3) pass through the pH value of addition sodium hydroxide or sulfuric acid adjusting black liquid concentrate to 8.5~12.5 in.
5. the method according to claim 1 for preparing sodium lignin sulfonate using black liquid, which is characterized in that the resistance
Poly- agent is one or more of epoxychloropropane, formic acid, acetic acid, sodium chloroacetate.
6. the method according to claim 1 for preparing sodium lignin sulfonate using black liquid, which is characterized in that step
(3) time-consuming that sodium sulfite is added in is 45 minutes~240 minutes.
7. the sodium lignin sulfonate that method described in any one of claim 1-6 obtains is used as dye dispersant.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112169753A (en) * | 2020-09-21 | 2021-01-05 | 张家港市杨舍丝印工艺厂 | Heavy metal adsorbent and preparation process thereof |
| CN113462195A (en) * | 2021-07-06 | 2021-10-01 | 浙江捷发科技股份有限公司 | Preparation method of modified sodium lignosulfonate dye dispersing agent |
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| CN102140173A (en) * | 2010-12-28 | 2011-08-03 | 新疆天宏纸业股份有限公司 | Method for producing sodium lignin sulfonate by using black liquor from pulping of reed containing sodium sulfite |
| CN102146164A (en) * | 2011-03-05 | 2011-08-10 | 福州大学 | Lignosulfonate prepared from ground wood pulp waste liquor and preparation process thereof |
| CN105601943A (en) * | 2015-11-13 | 2016-05-25 | 浙江捷发科技有限公司 | Method used for preparing sulfonated lignin from sulfate papermaking waste water |
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2018
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| US3966698A (en) * | 1975-05-02 | 1976-06-29 | Nalco Chemical Company | Recovery of tall oil soaps |
| CN102140173A (en) * | 2010-12-28 | 2011-08-03 | 新疆天宏纸业股份有限公司 | Method for producing sodium lignin sulfonate by using black liquor from pulping of reed containing sodium sulfite |
| CN102146164A (en) * | 2011-03-05 | 2011-08-10 | 福州大学 | Lignosulfonate prepared from ground wood pulp waste liquor and preparation process thereof |
| CN105601943A (en) * | 2015-11-13 | 2016-05-25 | 浙江捷发科技有限公司 | Method used for preparing sulfonated lignin from sulfate papermaking waste water |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112169753A (en) * | 2020-09-21 | 2021-01-05 | 张家港市杨舍丝印工艺厂 | Heavy metal adsorbent and preparation process thereof |
| CN112169753B (en) * | 2020-09-21 | 2023-08-29 | 北京伟创力科技股份有限公司 | Heavy metal adsorbent and preparation process thereof |
| CN113462195A (en) * | 2021-07-06 | 2021-10-01 | 浙江捷发科技股份有限公司 | Preparation method of modified sodium lignosulfonate dye dispersing agent |
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Application publication date: 20190226 |