CN102134404B - Modified lignin dispersant of disperse dye and preparation process thereof - Google Patents
Modified lignin dispersant of disperse dye and preparation process thereof Download PDFInfo
- Publication number
- CN102134404B CN102134404B CN 201110004571 CN201110004571A CN102134404B CN 102134404 B CN102134404 B CN 102134404B CN 201110004571 CN201110004571 CN 201110004571 CN 201110004571 A CN201110004571 A CN 201110004571A CN 102134404 B CN102134404 B CN 102134404B
- Authority
- CN
- China
- Prior art keywords
- parts
- disperse dye
- dispersant
- kilograms
- modified lignin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Phenolic Resins Or Amino Resins (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
Abstract
The invention relates to a modified lignin dispersant of a disperse dye and a preparation process thereof. The dispersant of the disperse dye comprises the following raw materials in parts by mass: 45.0-74.0 parts of pulping black liquid, 0.5-4.0 parts of oxidant, 3.0-8.0 parts of aldehydes, 0.5-5.4 parts of anion etherifying agent, 2.6-20.0 parts of amines, 8.0-18.0 parts of sulfonating agent and 10.0-30.0 parts of water. In the preparation process, black liquid produced in pulping industry is directly utilized to prepare the dispersant of the disperse dye, wherein the thermal stability of the dispersant at the temperatures of 130 DEG C and 150 DEG C is above level 4, the staining property of chinlon, terylene and cotton is above level 4, and the dispersion force of the dispersant is greater than 95%; on the basis that the cost of the product is greatly reduced, performances such as the dispersion force, the thermal stability and the like of the product are improved; the 'three wastes' are not discharged in the whole production process; and the high-value utilization of lignin is realized; and therefore, the preparation process is a clean and environment-friendly process.
Description
Technical field
The invention belongs to field of fine chemical, specially refer to a kind of modified lignin dispersant of disperse dye and preparation technology thereof.
Background technology
The world today, the deposit of oil, natural gas source is limited, and their research, development and utilization is on the rise to the impact that ball ecological environment brings, and this has impelled the macromolecular material take natural resource as raw material to be greatly developed.Xylogen is one of the abundantest, reproducible natural polymer child resource of occurring in nature.Whole world terrestrial plant can produce 50,000,000,000 tons of xylogen every year, and the industrial lignin that wherein produces in the cooking waste liquor of pulp and paper industry has 5,000 ten thousand tons.At present, the pulp and paper industry of China is take alkali and sulfate cooking slurrying as main, some large-scale enterprises in pulp and paper industry can be eliminated the rear recovery of black liquor of pulp making burning alkali lye by alkali recovery technology the pollution of black liquor of pulp making, but the method can cause the huge waste of Liginon Resource.Therefore xylogen is not also well utilized so far, China only approximately 6% xylogen utilized.How effectively to make good use of this renewable resources of xylogen, improve the starting point that its added value has become every researcher research.
Dispersed dye are the water-soluble lower nonionic dyes of a class.Be used for the earliest the dyeing of cellulose acetate fibre, be called cellulose acetate dye.Along with the development of synthon, polyamide fibre, terylene occur in succession, and dyestuff has been proposed Secretary.The domestic alone dispersion agent that waits the dyestuff post-treatment in reduction is estimated to want 6 ~ 100,000 tons every year.Good and bad quality and the whole dyeing course that directly affects dyestuff of dispersion agent, therefore, dispersion agent is very important.The dye dispersant that generally uses on the domestic and international market at present mainly contains several lower several types: (1) naphthalene sulfonic acidformaldehyde condensation product dispersion agent; (2) polycarboxylic acid series dispersion agent; (3) modified lignin resin class dispersion agent.
Wherein the heat-resistant stability of naphthalene sulfonic acidformaldehyde condensation product dispersion agent is not high, generally only have 120 ~ 130 ℃, its raw material (methylnaphthalene) can not meet the needs of production far away simultaneously, and product cost is higher, and then affect the price of naphthalene sulfonic acidformaldehyde condensation product dispersion agent product, thereby be unfavorable for that product applies in analyzing dyestuff.And the severe reaction conditions of polycarboxylic acid series dispersion agent, complex process, industrialization cost are high, and simultaneously, the monomer coverage rate of existing activity polymerizating technology is narrow, is mainly the monomers such as vinylbenzene, (methyl) esters of acrylic acid, and the designability of molecular structure is less.And modified lignin resin is mainly that as the advantage of dye dispersant (1) raw material sources are wide, and more easily obtaining, cost is lower simultaneously; (2) fuel system with numerous species has good compatible and good dispersing property.Xylogen also has the problem of some more difficult breakthroughs as dye dispersant, as dyeing and the heat-resistant stability thereof of xylogen to fiber but meanwhile.Overcoming of these difficult points become the focus that domestic and international expert competitively studies.
In recent years, the research of modified lignin resin dye dispersant was mainly concentrated on xylogen was carried out suitable chemically modified, to improve its performance, especially resistance toheat.Wang K C utilizes polyoxyethylene glycol ether epoxy EO-1, EO-2, EO-3 as dispersing auxiliary, can with the composite use of sulfonated lignin.But composite hydrophilic, lipophilic group and the surfactivity thereof that can not change in the lignosulfonic acid molecules of salt, and price is higher.Therefore, sulfonated lignin are carried out chemical modification, could prepare efficient modified lignin mahogany sulfonate dispersion agent (US 6066183).Dilling P utilizes V-Brite B to carry out pre-treatment to xylogen, then is reacted by S-WAT and aldehyde and modified lignin resin, to improve the thermotolerance (US 4338091) of xylogen.Wei Handaocai etc. are with electrooxidation and sulfomethylation method that physics and chemistry combines, provide a kind of reaction conditions gentle, do not produce public hazards, and the method (ZL 00131005.4) of the good preparing disperser by improving lignin of product dispersing property.
Therefore, if take xylogen as raw material, develop the modified lignin vat dye dispersing agent with certain sulfonation degree by chemical modification, not only greatly reduce the price of vat dye dispersing agent product, be conducive to applying of modified lignin vat dye dispersing agent, and will further widen the range of application of xylogen, and improve its added value, also improve simultaneously Enterprise Integrated and utilize xylogen and solve the enthusiasm that pulping back liquor pollutes, promote China's pulping and paper-making industry to continue, develop in a healthy way.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, it is poor to improve the added value of xylogen and solve traditional dispersant of disperse dye heat-resistant stability, and the high in cost of production problem provides a kind of modified lignin dispersant of disperse dye and preparation technology thereof.This technique is by directly utilizing the black liquor that produces in pulp industry, the preparation dispersant of disperse dye, with reduce or eliminate produce and use procedure in to the environment produced pollution, on the basis that greatly reduces product cost, improved the performances such as the dispersion force of product and heat-resistant stability.
The present invention implements by following technical solution:
A kind of raw material of modified lignin dispersant of disperse dye forms and mass fraction is:
Black liquor of pulp making: 45.0 parts～74.0 parts
Oxygenant: 0.5 part～4.0 parts
Aldehyde compound: 3.0 parts～8.0 parts
Negatively charged ion etherifying agent: 0.5 part～5.4 parts
Aminated compounds: 2.6 parts～20.0 parts
Sulphonating agent: 8.0 parts～18.0 parts
Water: 10.0 parts～30.0 parts.
The relative molecular mass of described dispersion agent is 3000 ~ 41000, is chocolate thick liquid or chocolate brown powder.
PH is 7.5～10.5 when the mass concentration of this aqueous dispersant is 1%.
More than 4 grades, polyamide fibre, terylene and cotton staining is more than 4 grades at the heat-resistant stability of 130 ℃ and 150 ℃ for described dispersion agent,
Dispersion force is greater than 95%.
This modified lignin dispersant of disperse dye preparation technology's concrete steps are:
Black liquor of pulp making and oxygenant are reacted 10～30min at the temperature of 40～95 ℃, add aldehyde compound, continue to be warming up to 90～160 ℃ after reaction 0.5～2 h, then add the reaction of negatively charged ion etherifying agent and aminated compounds to add the mixture of sulphonating agent and water after 0.5～1.5 h, after reaction 0.5～2 h, make described dispersion agent, prepared dispersion agent is chocolate liquid, by namely getting the brown solid powder after spraying drying; Above-mentioned preparation is to carry out under normal pressure.
The preparation method of described black liquor of pulp making is: select one or more in bamboo, bagasse, straw, wheat straw, hybrid giant napier, Stem of Lovely Achnatherum, Qu Liu, toothed oak wood, poplar, reed, Eucalyptus, birch, Pinus massoniana Lamb to prepare black liquor of pulp making by alkaline process or sulphate process, the solid content of black liquor is 8%～75%, wherein content of lignin is 9%～45%, and density is 1.13～1.51 g/ml.
Described oxygenant is one or more in potassium permanganate, hydrogen peroxide, potassium ferrate, sodium peroxide, Potassium Persulphate, Sodium Persulfate, ammonium persulphate, clorox.
Described aldehyde compound is formaldehyde, acetaldehyde, glutaraldehyde, propenal, succinic aldehyde, melamine formaldehyde (MF), trioxymethylene, in paraformaldehyde one or more.
Described negatively charged ion etherifying agent is one or more in oxyethane, propylene oxide, epoxy chloropropane, bromohexadecane, Monochloro Acetic Acid.
Described aminated compounds is one or more in dimethylamine, quadrol, thanomin, diethanolamine, trolamine, methane amide, ethanamide, diethylenetriamine, phenylenediamine.
Described sulphonating agent is one or more in S-WAT, inferior sour hydrogen sodium, chlorsulfonic acid, Sodium Pyrosulfite, sodium isethionate, ammonium sulphite, thionamic acid.
The invention has the advantages that:
1) the present invention mainly utilizes the by product in pulp industry---and xylogen is raw material, makes the product of developing have the low characteristics of cost.
2) the present invention is with the concentrated rear directly modification of black liquor of pulp making, need not reclaim modification again after xylogen by acidification, whole production process is discharged without " three wastes " (waste gas, waste water, waste residue), and solved the black liquor pollution problem of pulp and paper making, therefore this preparation technology be one clean, environmentally friendly technology, in the production cost that reduces product, also improved dispersiveness and the heat-resistant stability of product, there is not yet at present bibliographical information both at home and abroad.
3) the present invention adopts suitable oxygenant, etherifying agent and aminated compounds to carry out modification to xylogen, and improving the heat-resistant stability of dispersion agent, this product is combined the heat-resistant stability of rear 150 ℃ with vat dyes be more than level Four.
4) production technique of the present invention is simple, and raw materials for production are easy to get, and is with short production cycle, reaction temperature and, required equipment is conventional equipment, is convenient to existing chemical plant and practices midwifery.
Description of drawings
Fig. 1 is that dispersant of disperse dye is to the effect of 150 ℃ of heat-resistant stabilities of different dispersed dye;
Fig. 2 be under differing temps dispersant of disperse dye to dispersed dye heat-resistant stability on effect.
Embodiment
A kind of raw material of modified lignin dispersant of disperse dye forms and mass fraction is:
Black liquor of pulp making: 45.0 parts～74.0 parts
Oxygenant: 0.5 part～4.0 parts
Aldehyde compound: 3.0 parts～8.0 parts
Negatively charged ion etherifying agent: 0.5 part～5.4 parts
Aminated compounds: 2.6 parts～20.0 parts
Sulphonating agent: 8.0 parts～18.0 parts
Water: 10.0 parts～30.0 parts.
This modified lignin dispersant of disperse dye preparation technology's concrete steps are:
Black liquor of pulp making and oxygenant are reacted 10～30min at the temperature of 40～95 ℃, add aldehyde compound, continue to be warming up to 90～160 ℃ after reaction 0.5～2 h, then add the reaction of negatively charged ion etherifying agent and aminated compounds to add the mixture of sulphonating agent and water after 0.5～1.5 h, after reaction 0.5～2 h, make described dispersion agent, prepared dispersion agent is chocolate liquid, by namely getting the brown solid powder after spraying drying; Above-mentioned preparation is to carry out under normal pressure.
The preparation method of described black liquor of pulp making is: select one or more in bamboo, bagasse, straw, wheat straw, hybrid giant napier, Stem of Lovely Achnatherum, Qu Liu, toothed oak wood, poplar, reed, Eucalyptus, birch, Pinus massoniana Lamb to prepare black liquor of pulp making by alkaline process or sulphate process, the solid content of black liquor is 8%～75%, wherein content of lignin is 9%～45%, and density is 1.13～1.51 g/ml.
Described oxygenant is one or more in potassium permanganate, hydrogen peroxide, potassium ferrate, sodium peroxide, Potassium Persulphate, Sodium Persulfate, ammonium persulphate, clorox.
Described aldehyde compound is formaldehyde, acetaldehyde, glutaraldehyde, propenal, succinic aldehyde, melamine formaldehyde (MF), trioxymethylene, in paraformaldehyde one or more.
Described negatively charged ion etherifying agent is one or more in oxyethane, propylene oxide, epoxy chloropropane, bromohexadecane, Monochloro Acetic Acid.
Described aminated compounds is one or more in dimethylamine, quadrol, thanomin, diethanolamine, trolamine, methane amide, ethanamide, diethylenetriamine, phenylenediamine.
Described sulphonating agent is one or more in S-WAT, inferior sour hydrogen sodium, chlorsulfonic acid, Sodium Pyrosulfite, sodium isethionate, ammonium sulphite, thionamic acid.
Embodiment 1
1) raw material of the present embodiment and formula (unit-kilogram):
Alkaline process bamboo pulping black liquor (massfraction 75 %): 450.0 kilograms
Hydrogen peroxide: 5.0 kilograms
Formaldehyde: 60.0 kilograms
Oxyethane: 18.0 kilograms
Dimethylamine: 78.0 kilograms
S-WAT: 180.0 kilograms
Water: 209.0 kilograms
2) processing step and processing parameter
Preparation of the present invention is carried out under normal pressure:
first will be preheated to 40 ℃ in reactor, the black liquor of pulp making that adds the 450.0 kilogram-mass marks 45% that calculated, 5.0 kg peroxygen hydrogen, react 10 min, add 60.0 kilograms of formaldehyde, continue to be warming up to 90 ℃ after reaction 1 h, then add 18.0 kilograms of oxyethane, 78.0 kilogram dimethylamine, reaction 0.5h, the mixture that adds at last 180.0 kilograms of S-WATs and 209.0 kg water, after reacting 1.5 h, cooling discharge, prepared product is chocolate liquid, by namely getting the brown solid powder after spraying drying, adopt QZP-500 type Pressuresprayingdrier: 230 ℃ of spray tower inlet temperature, 80 ℃ of air outlet temperatures.The molecular weight of product is 17000.
Embodiment 2
1) raw material of the present embodiment and formula (unit-kilogram):
Alkaline pulping black liquor (bamboo and bagasse compound, quality proportioning are 6:4, and the concentrated black liquid solid content is 8%): 740.0 kilograms
Potassium permanganate: 10.0 kilograms
Acetaldehyde: 30.0 kilograms
Propylene oxide: 10.0 kilograms
Quadrol: 26.0 kilograms
Sodium Pyrosulfite: 80.0 kilograms
Water: 104.0 kilograms
2) processing step and processing parameter
Preparation of the present invention is carried out under normal pressure:
first will be preheated to 60 ℃ in reactor, the black liquor of pulp making that adds the 740.0 kilogram-mass marks 40% that calculated, 10.0 kilogram potassium permanganate, react 10 min, add 30.0 kilograms of acetaldehyde, continue to be warming up to 100 ℃ after reaction 0.5h, then add 10.0 kilograms of oxyethane, 26.0 kilogram quadrol, reaction 0.5h, the mixture that adds at last 80.0 kilograms of Sodium Pyrosulfites and 104.0 kg water, after reacting 1.5 h, cooling discharge, prepared product is chocolate liquid, by namely getting the brown solid powder after spraying drying, adopt LPG-150 type spray-dryer: 280 ℃ of spray tower inlet temperature, 120 ℃ of air outlet temperatures.The molecular weight of product is 9800.
Embodiment 3
1) raw material of the present embodiment and formula (unit-kilogram):
Alkaline pulping black liquor (bamboo and rice straw compound, the quality proportioning is 4:1, the black liquor solid content is 48%): 488.0 kilograms
Hydrogen peroxide: 20.0 kilograms
Potassium permanganate: 5.0 kilograms
Formaldehyde: 60.0 kilograms
Propenal: 20.0 kilograms
Monochloro Acetic Acid: 14.0 kilograms
Thanomin: 200.0 kilograms
Sodium Pyrosulfite: 60.0 kilograms
S-WAT: 20.0 kilograms
Water: 113.0 kilograms
2) processing step and processing parameter
Preparation of the present invention is carried out under normal pressure:
first will be preheated to 80 ℃ in reactor, the black liquor of pulp making that adds the 488.0 kilogram-mass marks 40% that calculated, 20.0 kg peroxygen hydrogen, 5.0 kilogram potassium permanganate, react 20 min, add 60.0 kilograms of formaldehyde, 20.0 kilogram propenal, continue to be warming up to 160 ℃ after reaction 1 h, then add 14.0 kilograms of Monochloro Acetic Acids, 200.0 kilogram thanomin, react 1 h, add at last 60.0 kilograms of Sodium Pyrosulfites, 20.0 the mixture of kilogram S-WAT and 113.0 kg water, after reacting 1 h, cooling discharge, prepared product is chocolate liquid, by namely getting the brown solid powder after spraying drying, adopt QZP-300 type Pressuresprayingdrier: 260 ℃ of spray tower inlet temperature, 105 ℃ of air outlet temperatures.The molecular weight of product is 3000.
Embodiment 4
1) raw material of the present embodiment and formula (unit-kilogram):
Alkaline pulping black liquor (bamboo and bagasse compound, quality proportioning are 1:1, black liquor solid content 67%): 558.0 kilograms;
Potassium Persulphate: 40.0 kilograms
Formaldehyde: 33.0 kilograms
Propenal: 11.0 kilograms
Epoxy chloropropane: 8.0 kilograms
Dimethylamine: 30.0 kilograms
Trolamine: 30.0 kilograms
Sodium bisulfite: 100.0 kilograms
Water: 190.0 kilograms
2) processing step and processing parameter
Preparation of the present invention is carried out under normal pressure:
first will be preheated to 95 ℃ in reactor, black liquor of pulp making and 40.0 kilograms of Potassium Persulphates of adding the 558.0 kilogram-mass marks 41% that calculated, react 30 min, add 33.0 kilograms of formaldehyde, 11.0 kilogram propenal, continue to be warming up to 140 ℃ after reaction 1.5 h, then add 8.0 kilograms of epoxy chloropropane, 30.0 kilogram dimethylamine, 30.0 kilogram trolamine, react 1 h, the mixture that adds at last 100.0 kilograms of sodium bisulfites and 190.0 kg water, after reacting 2 h, cooling discharge, prepared product is chocolate liquid, by namely getting the brown solid powder after spraying drying, 200 ℃ of spray tower inlet temperature, 110 ℃ of air outlet temperatures.The molecular weight of product is 41000.
Embodiment 5
1) raw material of the present embodiment and formula (unit-kilogram):
Alkaline process Eucalyptus black liquor of pulp making (55% solid content): 650.0 kilograms;
Potassium Persulphate: 12.0 kilograms
Potassium permanganate: 3.0 kilograms
Acetaldehyde: 21.0 kilograms
Propenal: 14.0 kilograms
Propylene oxide: 3.0 kilograms
Monochloro Acetic Acid: 2.0 kilograms
Methane amide: 100.0 kilograms
Sodium Pyrosulfite: 57.0 kilograms
S-WAT: 19.0 kilograms
Sodium bisulfite: 19.0 kilograms
Water: 100.0 kilograms
2) processing step and processing parameter
Preparation of the present invention is carried out under normal pressure:
first will be preheated to 90 ℃ in reactor, the black liquor of pulp making that adds the 650.0 kilogram-mass marks 55% that calculated, 12.0 kilogram Potassium Persulphate and 3.0 kilograms of potassium permanganate, react 30 min, add 21.0 kilograms of acetaldehyde, 14.0 kilogram propenal, continue to be warming up to 140 ℃ after reaction 2 h, then add 3.0 kilograms of epoxy chloropropane, 2.0 kilogram Monochloro Acetic Acid, 100.0 kilogram methane amide, react 1.5 h, add at last 57.0 kilograms of Sodium Pyrosulfites, 19.0 kilogram S-WAT, 19.0 the mixture of kilogram sodium bisulfite and 100.0 kg water, after reacting 2 h, cooling discharge, prepared product is chocolate liquid, by namely getting the brown solid powder after spraying drying, 230 ℃ of spray tower inlet temperature, 90 ℃ of air outlet temperatures.The molecular weight of product is 31300.
Embodiment 6
1) raw material of the present embodiment and formula (unit-kilogram):
Alkaline process Pinus massoniana Lamb black liquor of pulp making (46% solid content): 552.0 kilograms
Hydrogen peroxide: 24.0 kilograms
Potassium ferrate: 6.0 kilograms
Acetaldehyde: 54.0 kilograms
Oxyethane: 36.0 kilograms
Epoxy chloropropane: 18.0 kilograms
Diethanolamine: 28.0 kilograms
Quadrol: 56.0 kilograms
Chlorsulfonic acid: 102.0 kilograms
Water: 124.0 kilograms
2) processing step and processing parameter
Preparation of the present invention is carried out under normal pressure:
first will be preheated to 70 ℃ in reactor, the black liquor of pulp making that adds the 552.0 kilogram-mass marks 57% that calculated, 24.0 kg peroxygen hydrogen and 6.0 kilograms of potassium ferrates, react 30 min, add 54.0 kilograms of acetaldehyde, continue to be warming up to 140 ℃ after reaction 2 h, then add 36.0 kilograms of oxyethane, 18.0 kilogram epoxy chloropropane, 28.0 kilogram diethanolamine, 56.0 kilogram quadrol, react 1 h, the mixture that adds at last 102.0 kilograms of chlorsulfonic acids and 124.0 kg water, after reacting 0.5 h, cooling discharge, prepared product is chocolate liquid, by namely getting the brown solid powder after spraying drying, 230 ℃ of spray tower inlet temperature, 80 ℃ of air outlet temperatures).The molecular weight of product is 23200.
Embodiment 7
1) raw material of the present embodiment and formula (unit-kilogram):
Alkaline process birch black liquor of pulp making (52% solid content): 462.0 kilograms
Potassium ferrate: 8.0 kilograms
Trioxymethylene: 30.0 kilograms
Bromohexadecane: 10.0 kilograms
Quadrol: 65.0 kilograms
Chlorsulfonic acid: 125.0 kilograms
Water: 300.0 kilograms
2) processing step and processing parameter
Preparation of the present invention is carried out under normal pressure:
First will be preheated to 90 ℃ in reactor, black liquor of pulp making and 8.0 kilograms of potassium ferrates of adding the 462.0 kilogram-mass marks 52% that calculated, react 10 min, add 30.0 kilograms of trioxymethylenes to continue to be warming up to 100 ℃ after reaction 2 h, then the mixture that slowly adds 10.0 kilograms of bromohexadecanes, 65.0 kilograms of quadrols, 125.0 kilograms of chlorsulfonic acids and 300.0 kg water, after reaction 1h, cooling discharge, prepared product are chocolate liquid.The molecular weight of product is 19000.
Performance test
Heat-resistant stability detects and grades by HG/T 3507-2008 " sodium lignosulfonate dispersion agent " and HG/T 3399-2001 " mensuration of dye diffusion performance ".Details are seen Fig. 1, Fig. 2
The above is only preferred embodiment of the present invention, and all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (10)
1. modified lignin dispersant of disperse dye is characterized in that: the raw material of described dispersant of disperse dye forms and mass fraction is:
Black liquor of pulp making: 45.0 parts～74.0 parts
Oxygenant: 0.5 part～4.0 parts
Aldehyde compound: 3.0 parts～8.0 parts
Negatively charged ion etherifying agent: 0.5 part～5.4 parts
Aminated compounds: 2.6 parts～20.0 parts
Sulphonating agent: 8.0 parts～18.0 parts
Water: 10.0 parts～30.0 parts.
2. a kind of modified lignin dispersant of disperse dye according to claim 1, it is characterized in that: the relative molecular mass of described dispersion agent is 3000 ~ 41000, is chocolate thick liquid or chocolate brown powder.
3. a kind of modified lignin dispersant of disperse dye according to claim 1 is characterized in that: more than 4 grades, polyamide fibre, terylene and cotton staining are more than 4 grades at the heat-resistant stability of 130 ℃ and 150 ℃ for described dispersion agent, and dispersion force is greater than 95%.
4. modified lignin dispersant of disperse dye according to claim 1, it is characterized in that: the preparation method of described black liquor of pulp making is: select one or more in bamboo, bagasse, straw, wheat straw, hybrid giant napier, Stem of Lovely Achnatherum, Qu Liu, toothed oak wood, poplar, reed, Eucalyptus, birch, Pinus massoniana Lamb to prepare black liquor of pulp making by alkaline process or sulphate process, the solid content of black liquor is 8%～75%, wherein content of lignin is 9%～45%, and density is 1.13～1.51 g/mL.
5. modified lignin dispersant of disperse dye according to claim 1, it is characterized in that: described oxygenant is one or more in potassium permanganate, hydrogen peroxide, potassium ferrate, sodium peroxide, Potassium Persulphate, Sodium Persulfate, ammonium persulphate, clorox.
6. modified lignin dispersant of disperse dye according to claim 1, it is characterized in that: described aldehyde compound is formaldehyde, acetaldehyde, glutaraldehyde, propenal, succinic aldehyde, melamine formaldehyde (MF), trioxymethylene, in paraformaldehyde one or more.
7. modified lignin dispersant of disperse dye according to claim 1, it is characterized in that: described negatively charged ion etherifying agent is one or more in oxyethane, propylene oxide, epoxy chloropropane, bromohexadecane, Monochloro Acetic Acid.
8. modified lignin dispersant of disperse dye according to claim 1, it is characterized in that: described aminated compounds is one or more in dimethylamine, quadrol, thanomin, diethanolamine, trolamine, methane amide, ethanamide, diethylenetriamine, phenylenediamine.
9. modified lignin dispersant of disperse dye according to claim 1, it is characterized in that: described sulphonating agent is one or more in S-WAT, chlorsulfonic acid, Sodium Pyrosulfite, sodium isethionate, ammonium sulphite, thionamic acid.
10. the preparation technology of a modified lignin dispersant of disperse dye as claimed in claim 1, it is characterized in that: described preparation technology's concrete steps are:
Black liquor of pulp making and oxygenant are reacted 10～30min at the temperature of 40～95 ℃, add aldehyde compound, continue to be warming up to 90～160 ℃ after reaction 0.5～2 h, then add the reaction of negatively charged ion etherifying agent and aminated compounds to add the mixture of sulphonating agent and water after 0.5～1.5 h, after reaction 0.5～2 h, make described dispersion agent, prepared dispersion agent is chocolate liquid, by namely getting the brown solid powder after spraying drying; Above-mentioned preparation is to carry out under normal pressure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110004571 CN102134404B (en) | 2011-01-11 | 2011-01-11 | Modified lignin dispersant of disperse dye and preparation process thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110004571 CN102134404B (en) | 2011-01-11 | 2011-01-11 | Modified lignin dispersant of disperse dye and preparation process thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102134404A CN102134404A (en) | 2011-07-27 |
| CN102134404B true CN102134404B (en) | 2013-05-08 |
Family
ID=44294343
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110004571 Active CN102134404B (en) | 2011-01-11 | 2011-01-11 | Modified lignin dispersant of disperse dye and preparation process thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102134404B (en) |
Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643309B (en) * | 2012-04-06 | 2014-04-23 | 大连工业大学 | Novel dye dispersant and preparation method thereof |
| CN103131020B (en) * | 2013-01-22 | 2015-04-22 | 华南理工大学 | Carboxylic sulfonic-acid-group lignin dye dispersing agent and preparation method thereof |
| CN103275520B (en) * | 2013-05-30 | 2014-06-04 | 金华双宏化工有限公司 | Preparation method of complex leather dye |
| CN103602237B (en) * | 2013-11-19 | 2016-08-17 | 青岛祥嘉知识产权服务有限公司 | A kind of waterproof coating |
| CN103755211A (en) * | 2013-12-16 | 2014-04-30 | 华南理工大学 | Papermaking black liquid modification admixture for impervious mortar and preparation method thereof |
| CN104530756B (en) * | 2014-10-20 | 2016-06-01 | 华南理工大学 | A kind of Lignins nano-dispersed dye well its preparation method |
| CN106432750B (en) * | 2016-09-12 | 2018-11-23 | 福州大学 | The method that capacitive deionization method purifying black liquor of pulp making prepares lignin-base dispersing agent |
| CN109503221B (en) * | 2018-11-13 | 2021-10-22 | 金正大生态工程集团股份有限公司 | Modified lignin chelated fertilizer and preparation method thereof |
| CN110078877B (en) * | 2019-04-26 | 2021-07-27 | 福州大学 | Method for preparing dispersant by using lignin degradation product and application |
| CN111847817B (en) * | 2020-09-01 | 2022-11-11 | 广西大学 | Oil sludge demulsifier, preparation method and application thereof |
| CN112760089B (en) * | 2021-01-28 | 2022-10-14 | 重庆化工职业学院 | Lignin-based gemini surfactant and preparation method thereof |
| CN118489689A (en) * | 2024-07-19 | 2024-08-16 | 山东中新科农生物科技有限公司 | Carbendazim wettable powder and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4338091A (en) * | 1981-08-13 | 1982-07-06 | Westvaco Corporation | Process for lowering the viscosity of sulfonated lignins |
| US6066183A (en) * | 1998-04-13 | 2000-05-23 | I-Hwa Industrial Co., Ltd. | Liquid dispersed dye of the azo or anthraquinone type |
| CN1911828A (en) * | 2005-08-10 | 2007-02-14 | 福州大学 | Modified lignin oil removing flocculant and its preparation method |
| CN101225336A (en) * | 2008-02-01 | 2008-07-23 | 福州大学 | Alkali lignin-sulphonated acetone formaldehyde polycondensates coal water slurry additive and preparation method thereof |
| CN101224958A (en) * | 2008-02-01 | 2008-07-23 | 福州大学 | Sulfonated alkali lignin modified sulfamate high-effective water reducer and preparation method thereof |
| CN101474543A (en) * | 2008-12-30 | 2009-07-08 | 浙江龙盛染料化工有限公司 | Preparation method of composite dispersant |
-
2011
- 2011-01-11 CN CN 201110004571 patent/CN102134404B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4338091A (en) * | 1981-08-13 | 1982-07-06 | Westvaco Corporation | Process for lowering the viscosity of sulfonated lignins |
| US6066183A (en) * | 1998-04-13 | 2000-05-23 | I-Hwa Industrial Co., Ltd. | Liquid dispersed dye of the azo or anthraquinone type |
| CN1911828A (en) * | 2005-08-10 | 2007-02-14 | 福州大学 | Modified lignin oil removing flocculant and its preparation method |
| CN101225336A (en) * | 2008-02-01 | 2008-07-23 | 福州大学 | Alkali lignin-sulphonated acetone formaldehyde polycondensates coal water slurry additive and preparation method thereof |
| CN101224958A (en) * | 2008-02-01 | 2008-07-23 | 福州大学 | Sulfonated alkali lignin modified sulfamate high-effective water reducer and preparation method thereof |
| CN101474543A (en) * | 2008-12-30 | 2009-07-08 | 浙江龙盛染料化工有限公司 | Preparation method of composite dispersant |
Non-Patent Citations (4)
| Title |
|---|
| 亚铵法草浆废液固氮技术及木质素磺酸盐结构与性能的规律;王哲;《南京林业大学 博士学位论文》;20081007;3-20 * |
| 方桂珍.超声波活化碱木质素及多效碱木质素水处理剂合成与应用研究.《东北林业大学 博士学位论文》.2006, |
| 王哲.亚铵法草浆废液固氮技术及木质素磺酸盐结构与性能的规律.《南京林业大学 博士学位论文》.2008, |
| 超声波活化碱木质素及多效碱木质素水处理剂合成与应用研究;方桂珍;《东北林业大学 博士学位论文》;20060613;1-16 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102134404A (en) | 2011-07-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102134404B (en) | Modified lignin dispersant of disperse dye and preparation process thereof | |
| CN102078780B (en) | Modified lignin vat dye dispersing agent and preparation process thereof | |
| CN102604120B (en) | Method for preparing lignin sulfonate dispersing agent by using two-step oxidization method | |
| CN102690423B (en) | Method for producing sodium lignosulphonate by utilizing residues obtained by producing ethanol with crop straws as raw materials | |
| WO2014114155A1 (en) | Lignin dye dispersant with carboxyl and sulfonic groups and preparation method therefor | |
| CN102441339B (en) | Dissolving pulp sodium lignosulfonate dispersant, and reducing preparation method and application thereof | |
| WO2020215561A1 (en) | Method and application for preparing dispersant using lignin degradation product | |
| CN102146164B (en) | Lignosulfonate prepared from ground wood pulp waste liquor and preparation process thereof | |
| CN102153764B (en) | Method for preparing lignin sodium sulfonate dispersant through advanced catalytic oxidation | |
| CN106750179B (en) | A kind of preparation method of enzymolysis xylogen base epoxy | |
| CN104474966A (en) | Modified lignin-based dispersing agent and preparation method thereof | |
| CN107362810A (en) | A kind of magnetic mao bamboon charcoal solid acid catalyst and preparation method and its application in xylo-oligosaccharide is prepared | |
| CN104672469B (en) | A kind of quaternized lignin-base dispersant and preparation technology and application | |
| CN103319738B (en) | The method that agricultural crop straw prepares regenerated cellulose composite film | |
| CN109679113A (en) | A kind of preparation method of low contamination lignosulfonates | |
| CN104356689A (en) | Low-pollution lignin dispersant for disperse dye as well as preparation method and application thereof | |
| CN104592529A (en) | Novel lignin sulfonation technology | |
| CN110483807A (en) | A kind of method that soda spent liquor prepares ligno-sulfate based plasticizer | |
| CN108276587B (en) | Method for preparing lignosulfonate by using pipeline reaction device | |
| CN103497342B (en) | A kind of method of producing enzymolysis xylogen sulfonate | |
| CN104785162B (en) | A kind of amine-methylated lignin-base dispersant and preparation technology and application | |
| CN103045678A (en) | Comprehensive utilization method of lignocellulose biomass | |
| CN102503990B (en) | Method for preparing surfactant by taking lignin thermo-chemically degraded phenol product as raw material | |
| CN111454139A (en) | Method for preparing formic acid by vanadium and sulfuric acid efficient circulating catalysis of biomass through trace DMSO (dimethyl sulfoxide) | |
| CN108864442A (en) | A method of lignosulphonates are prepared using dissolving pulp pre-cooked waste liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |