CN112521623A - Lignin emulsifier, asphalt emulsifier, preparation method of asphalt emulsifier and asphalt - Google Patents

Lignin emulsifier, asphalt emulsifier, preparation method of asphalt emulsifier and asphalt Download PDF

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CN112521623A
CN112521623A CN201911396460.XA CN201911396460A CN112521623A CN 112521623 A CN112521623 A CN 112521623A CN 201911396460 A CN201911396460 A CN 201911396460A CN 112521623 A CN112521623 A CN 112521623A
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emulsifier
asphalt
lignin
solution
imidazoline
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唐地源
江成真
韩文彬
张燕
高绍丰
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Jinan Shengquan Group Share Holding Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08HDERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H6/00Macromolecular compounds derived from lignin, e.g. tannins, humic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/02Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L95/00Compositions of bituminous materials, e.g. asphalt, tar, pitch
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L97/00Compositions of lignin-containing materials
    • C08L97/005Lignin
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2395/00Bituminous materials, e.g. asphalt, tar or pitch
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2463/00Characterised by the use of epoxy resins; Derivatives of epoxy resins
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2497/00Characterised by the use of lignin-containing materials
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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Abstract

The invention discloses a lignin emulsifier, an asphalt emulsifier, a preparation method thereof and asphalt, wherein the preparation method of the lignin emulsifier comprises the following steps: adding deionized water into lignin, adding sodium hydroxide, a hydrogen peroxide solution and cuprous sulfate to obtain a mixed solution, reacting the mixed solution at 80-120 ℃ for 1-3 h, adding a sodium hydroxide solution, and adjusting the pH value of the mixed solution to 9-12; cooling to 20-25 ℃, adding amine substances to react for 0.1-2 h, adding a formaldehyde solution, heating to 80-100 ℃, and continuing to react for 2-5 h to generate a lignin emulsifier; the asphalt emulsifier comprises the following components: the lignin emulsifier, the imidazoline cationic emulsifier, the alkylphenol ethoxylate, the inorganic salt and the water-based epoxy resin prepared by the method. The asphalt emulsifier has good adaptability to asphalt, can realize the emulsification of matrix asphalt and modified asphalt, has good storage stability, makes up the defect of single emulsifier, has simple preparation process, and is suitable for industrial production.

Description

Lignin emulsifier, asphalt emulsifier, preparation method of asphalt emulsifier and asphalt
Technical Field
The invention belongs to the field of asphalt, and particularly relates to a lignin emulsifier, an asphalt emulsifier, a preparation method of the lignin emulsifier and asphalt.
Background
In recent years, the construction of expressway in China is vigorously developed, the emulsified asphalt is widely applied with excellent performance, and the most key point for preparing the emulsified asphalt is the emulsifier.
The emulsifiers are mainly classified into cationic emulsifiers, anionic emulsifiers and nonionic emulsifiers. The cationic emulsifier is the most widely used emulsifier at present, and has good adaptability to stone and asphalt. The anionic emulsifier has high requirements on water quality and stone materials, so that the application of the anionic emulsifier is limited. The nonionic emulsifier has a good emulsifying effect but poor storage stability. The emulsifier of a single variety is difficult to realize the application requirements of different types of asphalt and different stones, and most of the conventional emulsifiers only aim at the base asphalt and have poor emulsification effects on SBS modified asphalt, SBR modified asphalt and SIS modified asphalt. The composite asphalt emulsifier can make up the deficiency of a single emulsifier, and has good emulsifying effect on both the matrix asphalt and the modified asphalt.
The existing emulsifier is mostly used for emulsifying base asphalt, and the emulsifier for SBS modified asphalt is less, but the emulsifying performance of the emulsifier for SBS modified asphalt in the prior art does not reach the expected period.
The prior art discloses a double-Y type liquid fast-cracking cationic emulsifier for SBS modified asphalt emulsification and application thereof, wherein the molecular structural formula is as follows:
Figure BDA0002346452510000011
wherein R1 has the formula CnHmWherein m is 2n +1, 2n-3 or 2n-5, the emulsifier is liquid at normal temperature and can emulsify SBS modified asphalt, but the emulsifying performance of the emulsifier for emulsifying SBS modified asphalt is not superior and is not expected. Based on the problem, it is very practical to develop an emulsifier for emulsifying modified asphalt.
Disclosure of Invention
In order to solve the problems of the prior art, an object of the present invention is to provide a method for preparing a lignin emulsifier, comprising the steps of: adding deionized water into lignin, adding sodium hydroxide, a hydrogen peroxide solution and cuprous sulfate to obtain a mixed solution, reacting the mixed solution at 80-120 ℃ for 1-3 h, adding a sodium hydroxide solution, and adjusting the pH value of the mixed solution to 9-12; cooling to 20-25 ℃, adding amine substances to react for 0.1-2 h, adding formaldehyde, heating to 80-100 ℃, and continuing to react for 2-5 h to generate the lignin emulsifier. Among them, lignin can be derived from black liquor produced in the pulp and paper industry or from a by-product of sulfite process paper making.
Further, the amine substance can be one or a mixture of at least two of triethylene tetramine, tetraethylene pentamine, diethylene triamine and hydroxyethyl ethylene diamine; the mass ratio of the amine substance to the lignin in an oven-dry state can be 0.1-0.3: 1; the molar ratio of the amine substance to the formaldehyde can be 1: 1-5; the mass ratio of the cuprous sulfate to the lignin in an oven-dry state can be 0.01-0.05: 1.
Further, the mass concentration of the sodium hydroxide solution can be 10% -40%, and the mass ratio of the sodium hydroxide in an oven-dry state to the lignin in an oven-dry state can be 0.1-0.3: 1.
Furthermore, the concentration of the hydrogen peroxide solution can be 0.5-3.5 mol/L, and the mass ratio of hydrogen peroxide contained in the hydrogen peroxide solution to lignin in an absolutely dry state can be 0.001-0.007: 1.
It is another object of the present invention to provide a lignin emulsifier prepared by one of the above methods.
Another object of the present invention is to provide a bitumen emulsifier, which comprises the following components: the lignin emulsifier, the imidazoline cationic emulsifier, the alkylphenol epoxy vinyl ether, the inorganic salt and the water-based epoxy resin are provided.
Furthermore, the imidazoline cationic emulsifier can comprise an imidazoline emulsifier with a long-chain alkyl group and 14-18 carbon atoms; the alkylphenol epoxy vinyl ether can be an alkylphenol epoxy vinyl ether emulsifier with the hydrophilic-lipophilic balance value within the range of 12-18, and the alkylphenol epoxy vinyl ether emulsifier can comprise one or a mixture of at least two of OP series emulsifier, NP series emulsifier and TX series emulsifier; the OP series emulsifier can be one or a mixture of at least two of OP-9, OP-10, OP-13, OP-1, OP-20 and OP-30; the inorganic salt may be selected from one or a mixture of at least two of calcium chloride, sodium chloride, ammonium chloride, sodium sulfate, calcium sulfate, and ferric chloride.
Further, the mass percentages of the lignin emulsifier, the imidazoline cationic emulsifier, the alkylphenol ethylene oxide ether, the inorganic salt and the water-based epoxy resin are respectively 30-70%, 5-25%, 20-65%, 0.2-5% and 1-5%.
Another object of the present invention is to provide a method for preparing the asphalt emulsifier, which comprises the following steps: adding a lignin emulsifier, an imidazoline cationic emulsifier and alkylphenol ethoxylates into a device with reflux condensation, heating to 50-90 ℃, and stirring for 1-5 h; cooling to 20-40 ℃, adding aqueous epoxy resin and inorganic salt into the device, and continuously stirring for 1-2 h to generate the asphalt emulsifier.
It is another object of the present invention to provide a bitumen comprising the above bitumen emulsifier.
The asphalt emulsifier provided by the invention has good adaptability to asphalt, can realize emulsification of matrix asphalt and modified asphalt, has good storage stability, makes up for the defect of a single emulsifier, has a simple preparation process, and is suitable for industrial production.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
Furthermore, the terms "including" and "having," as well as any variations thereof, are intended to cover non-exclusive inclusions. For example, a process, method, system, article, or apparatus that comprises a list of steps or elements is not limited to only those steps or elements listed, but may alternatively include other steps or elements not listed, or inherent to such process, method, article, or apparatus.
Reference herein to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment can be included in at least one embodiment of the application. The appearances of the phrase in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. Those skilled in the art will explicitly and implicitly appreciate that the embodiments described herein may be combined with other embodiments.
In the following experiments, the information on the source and purity of the main raw materials used is shown in table 1.
Table 1: the source and purity of the main raw materials
Figure BDA0002346452510000041
Figure BDA0002346452510000051
Preparation of lignin emulsifier
Preparation example 1
500g of lignin and 500g of deionized water are added into a four-mouth bottle, 170g of sodium hydroxide solution with the mass fraction of 30 percent is slowly added after stirring, 5g of copper sulfite and 10ml of 1.5mol/L hydrogen peroxide solution are added for reaction at the temperature of 80 ℃ for 1 hour, and 1mol/L sodium hydroxide solution is added to adjust the pH value of the solution to 10.0. Cooling to 20 ℃, adding 0.5mol of triethylene tetramine (73.115 g of triethylene tetramine) and formaldehyde solution (the mass concentration is 40 percent, namely 75g of formaldehyde solution) containing 1mol of formaldehyde, heating to 100 ℃, and continuously reacting for 3 hours to obtain the lignin emulsifier.
Preparation example 2
500g of lignin and 500g of deionized water are added into a four-mouth bottle, 200g of sodium hydroxide solution with the mass fraction of 30% is slowly added after stirring is started, 10g of copper sulfite and 15ml of 1.5mol/L hydrogen peroxide solution are added, the mixture reacts for 1 hour at the temperature of 80 ℃, and 1mol/L sodium hydroxide solution is added to adjust the pH value of the solution to 10.0. Cooling to 20 ℃, adding 0.75mol of triethylene tetramine (109.673 g of triethylene tetramine) and formaldehyde solution (the mass concentration is 40 percent, namely 112,5g of formaldehyde solution) containing 1.5mol of formaldehyde, heating to 100 ℃, and continuously reacting for 5h to obtain the lignin emulsifier.
Preparation of asphalt emulsifier
The lignin emulsifiers in the following examples were all the lignin emulsifiers obtained in preparation example 1.
Example 1
An asphalt emulsifier comprises the following raw materials in mass: 50g of lignin emulsifier, 10g of imidazoline emulsifier and OP-1035 g of alkylphenol polyoxyethylene ether, wherein the HLB (hydrophilic-Lipophilic Balance) value of OP-10 is 14, 4g of water-based epoxy resin and CaCl2 1g。
The preparation method comprises the steps of adding the lignin emulsifier, the imidazoline emulsifier and the alkylphenol polyoxyethylene OP-10 in the raw materials into a device with reflux condensation, heating to 60 ℃, and stirring for 4 hours. DescendHeating to 25 deg.C, adding aqueous epoxy resin and CaCl2And continuously stirring for 1 hour to obtain the asphalt emulsifier.
Example 2
An asphalt emulsifier comprises the following raw materials in mass: 45g of lignin emulsifier, 5g of imidazoline emulsifier, OP-1047 g of alkylphenol polyoxyethylene, 2.8g of aqueous epoxy resin, CaCl2 0.2g。
The preparation method comprises the steps of adding the lignin emulsifier, the imidazoline emulsifier and the alkylphenol polyoxyethylene OP-10 in the raw materials into a device with reflux condensation, heating to 80 ℃, and stirring for 3 hours. Cooling to 25 ℃, adding aqueous epoxy resin and CaCl2And continuously stirring for 2 hours to obtain the asphalt emulsifier.
Example 3
An asphalt emulsifier comprises the following raw materials in mass: 65g of lignin emulsifier, 10g of imidazoline emulsifier, OP-1022 g of alkylphenol polyoxyethylene, 1g of water-based epoxy resin and NH4Cl 2g。
The preparation method comprises the steps of adding the lignin emulsifier, the imidazoline emulsifier and the alkylphenol polyoxyethylene OP-10 in the raw materials into a device with reflux condensation, heating to 90 ℃, and stirring for 2 hours. Cooling to 25 ℃, adding water-based epoxy resin and NH4And Cl, and continuously stirring for 1h to obtain the asphalt emulsifier.
Example 4
An asphalt emulsifier comprises the following raw materials in mass: 30g of lignin emulsifier, 25g of imidazoline emulsifier, OP-1044 g of alkylphenol polyoxyethylene, 0.5g of aqueous epoxy resin, CaCl2 0.5g。
The preparation method comprises the steps of adding the lignin emulsifier, the imidazoline emulsifier and the alkylphenol polyoxyethylene OP-10 in the raw materials into a device with reflux condensation, heating to 90 ℃, and stirring for 2 hours. Cooling to 25 ℃, adding aqueous epoxy resin and CaCl2And continuously stirring for 1 hour to obtain the asphalt emulsifier.
Example 5
An asphalt emulsifier comprises the following raw materials in mass: 30g of lignin emulsifier, 5g of imidazoline emulsifier and OP-1060 g of alkylphenol polyoxyethylene4g of aqueous epoxy resin, Na2SO4 1g。
The preparation method comprises the steps of adding the lignin emulsifier, the imidazoline emulsifier and the alkylphenol polyoxyethylene OP-10 in the raw materials into a device with reflux condensation, heating to 90 ℃, and stirring for 2 hours. Cooling to 25 ℃, adding water-based epoxy resin and Na2SO4And continuously stirring for 1 hour to obtain the asphalt emulsifier.
Comparative example 1
Compared with the example 1, the difference is that the lignin emulsifier is replaced by octadecyl propylene diamine, and the rest is the same, and the description is not repeated.
The octadecyl propylene diamine has the performance similar to that of a lignin emulsifier, and is commonly used as a raw material for preparing emulsified asphalt.
Preparation of emulsified asphalt
Application example 1
Weighing 10g of the emulsifier prepared in example 1, adding water to 300g to obtain a soap solution, adjusting the pH of the soap solution to 2.0 by using hydrochloric acid (wherein the concentration of the hydrochloric acid is not limited), continuously adding water until the total mass of the soap solution is 350g, and heating to 60 ℃. Weighing 650g of Qilu 70# asphalt, heating to 130-150 ℃, and preparing the emulsified asphalt by the soap solution and the asphalt through a colloid mill.
Application example 2
Compared with application example 1, the difference is that the dosage of the emulsifier is 5g, and the rest is the same, so the description is not repeated.
Application example 3
Compared with application example 1, the difference is that the dosage of the emulsifier is 15g, and the rest is the same, so the description is not repeated.
Application example 4
Compared with application example 1, the difference is that the dosage of the emulsifier is 25g, and the rest is the same, so the description is not repeated.
Application example 5
Compared with application example 1, the difference is that the pH of the soap solution is adjusted to 2.5, and the rest is the same, and detailed description is omitted.
Application example 6
Compared with application example 1, the difference is that the pH of the soap solution is adjusted to 2.8, and the rest is the same, and detailed description is omitted.
Application example 7
Compared with the application example 1, the asphalt is SBS modified asphalt, wherein the SBS type of the SBS asphalt is YH-4303, and the mixing amount of the SBS asphalt is 3%, and the preparation method comprises the steps of weighing 19.5g of SBS modifier, adding the SBS modifier into 650g of Qilu 70# asphalt which is preheated to 170-180 ℃, shearing at a high speed of 8000rpm for 60min, and then developing at 170-180 ℃ for 60min to obtain the SBS modified asphalt.
And (3) preparing the emulsified asphalt by using the soap solution in the application example 1 and the prepared SBS modified asphalt through a colloid mill.
Application example 8
Compared with application example 7, the difference is that the zilu 70# asphalt is replaced by zilu 90# asphalt, and the rest is the same, and the description is omitted.
Application example 9
Compared with application example 7, the difference is that zilu 70# asphalt is replaced by zhonghai oil 70# asphalt, and the rest is the same, so that the description is omitted.
Application example 10
Compared with application example 7, the difference is that zilu 70# asphalt is replaced by SK70# asphalt, and the rest is the same and is not described again.
Comparative example 1
Compared with the application example 1, the emulsifying agent adopts octadecylamine, the rest is the same, and the description is omitted, wherein the octadecylamine is a conventional asphalt emulsifying agent.
Comparative example 2
Compared with the comparative example 1, the asphalt is the SBS modified asphalt prepared in the application example 7, and the rest is the same, so that the detailed description is omitted.
Comparative example 3
Compared with application example 1, the asphalt emulsifier prepared in comparative example 1 is used as the emulsifier, and the rest is the same and is not described again.
Comparative example 4
Compared with the comparative example 3, the asphalt is the SBS modified asphalt prepared in the application example 7, and the rest is the same, so that the detailed description is omitted.
Comparative example 5
Compared with application example 1, the emulsifier is a double-Y type liquid fast-cracking cationic emulsifier described in the background art, namely a liquid amine emulsifier in Table 1, and the rest are the same and are not repeated.
Wherein, the molecular structural formula of the liquid amine emulsifier is as follows:
Figure BDA0002346452510000091
wherein the molecular formula of R1 in the molecular structural formula is CnHmWherein N is a natural number of 12-18, M is 2N +1, 2N-3 or 2N-5, X and M are both N, R2 is a straight chain C3H6R3 is straight chain C2H5O, R4 are straight chain C2H5O, R5 are straight chain C2H5O。
Comparative example 6
Compared with the comparative example 5, the asphalt used is the SBS modified asphalt prepared in the application example 7, and the rest is the same, so that the description is omitted.
The detection method of the emulsified asphalt is carried out according to road engineering asphalt and asphalt mixture test procedure JTG E20-2011.
Table 2: performance results of the emulsified asphalt prepared in each application example and comparative example
Figure RE-GDA0002467620710000101
Figure BDA0002346452510000111
As shown in Table 2, the properties of the emulsified asphalt prepared in the application example were not greatly different from those of the emulsified asphalt prepared in the comparative example except for the storage stability, and all the properties had reached the acceptable standards. The most important property of the emulsified asphalt is storage stability, because other properties besides storage stability can be modified by adding additives.
According to the standard, the difference of 1d in storage is not more than 1%, and the difference of 5d in storage is not more than 5%, which indicates whether the emulsifying property of the asphalt emulsifier can be maintained for a long time.
It can be seen that the storage stability of the emulsified asphalt prepared by the emulsified unmodified asphalt in the application examples 1 to 6 and the comparative examples 1, 3 and 5 reaches the standard values in both 1d and 5 d.
The emulsified asphalt prepared by the emulsified SBS modified asphalt of the comparative example 2 and the comparative example 4 has obviously failed standards of 1d and 5d storage stability, and has very obvious difference.
Comparative example 6, which emulsifies SBS modified asphalt with emulsifier provided in the prior art, it can be seen that the storage stability of the emulsified asphalt reaches the standard, but the 5d storage stability reaches 4.76%, and the upper limit difference of the distance 5% is not large. The application examples 7-10 are all prepared by emulsifying SBS modified asphalt, and it can be seen that the storage stability of the asphalt emulsifier emulsified modified asphalt prepared by the method is obviously superior to that of the prior art, the storage stability of the asphalt emulsifier emulsified modified asphalt prepared by the method is about 2.5% in 5 days, wherein the maximum is 2.81%, and the minimum is 2.34%.
In conclusion, the asphalt emulsifier provided by the invention can be used for emulsifying not only common asphalt but also modified asphalt, which shows that the asphalt emulsifier provided by the invention has obvious advantages in the emulsification of modified asphalt, and the prepared emulsified asphalt has more excellent storage stability.
It should be understood that the above examples are only for clearly illustrating the present application and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of this invention may be made without departing from the spirit or scope of the invention.

Claims (10)

1. The preparation method of the lignin emulsifier is characterized by comprising the following steps:
adding deionized water into lignin, adding sodium hydroxide, a hydrogen peroxide solution and cuprous sulfate to obtain a mixed solution, reacting the mixed solution at 80-120 ℃ for 1-3 h, and adding a sodium hydroxide solution to adjust the pH of the mixed solution to 9-12;
cooling to 20-25 ℃, adding amine substances to react for 0.1-2 h, adding formaldehyde solution, heating to 80-100 ℃, and continuing to react for 2-5 h to generate the lignin emulsifier.
2. The method according to claim 1, wherein the amine is one or a mixture of at least two selected from the group consisting of triethylene tetramine, tetraethylene pentamine, diethylene triamine and hydroxyethyl ethylene diamine;
the mass ratio of the amine substance to the lignin in an oven-dry state is 0.1-0.3: 1;
the molar ratio of the amine substance to the formaldehyde is 1: 1-5;
the mass ratio of the cuprous sulfate to the lignin in an oven-dry state is 0.01-0.05: 1.
3. The method according to claim 1, wherein the concentration of the sodium hydroxide solution is 10-40%, and the mass ratio of the sodium hydroxide in an oven-dried state to the lignin in an oven-dried state is 0.1-0.3: 1.
4. The method according to claim 1, wherein the concentration of the hydrogen peroxide solution is 0.5 to 3.5mol/L, and the mass ratio of hydrogen peroxide contained in the hydrogen peroxide solution to the lignin in an absolutely dry state is 0.001 to 0.007: 1.
5. A lignin-based emulsifier prepared by the method of any one of claims 1 to 4.
6. An asphalt emulsifier, wherein the emulsifier comprises: the lignin emulsifier, the imidazoline based cationic emulsifier, the alkylphenol ethoxylate, the inorganic salt, and the aqueous epoxy resin of claim 5.
7. The asphalt emulsifier of claim 6, wherein the imidazoline based cationic emulsifier comprises an imidazoline emulsifier having 14 to 18 carbon atoms in a long chain alkyl group;
the alkylphenol ethoxylate is alkylphenol ethoxylate emulsifier with a hydrophilic-lipophilic balance value within the range of 12-18, the alkylphenol ethoxylate emulsifier comprises one or a mixture of at least two of OP series emulsifier, NP series emulsifier and TX series emulsifier, and the OP series emulsifier is selected from one or a mixture of at least two of OP-9, OP-10, OP-13, OP-1, OP-20 and OP-30;
the inorganic salt is selected from one or a mixture of at least two of calcium chloride, sodium chloride, ammonium chloride, sodium sulfate, calcium sulfate and ferric chloride.
8. The asphalt emulsifier of claim 6, wherein the mass percentages of the lignin emulsifier, the imidazoline based cationic emulsifier, the alkylphenol ethoxylate, the inorganic salt, and the aqueous epoxy resin are 30-70%, 5-25%, 20-65%, 0.2-5%, and 1-5%, respectively.
9. A preparation method of the asphalt emulsifier according to any one of claims 6 to 8, characterized by comprising the following steps:
adding the lignin emulsifier, the imidazoline cationic emulsifier and the alkylphenol ethoxylates into a device with reflux condensation, heating to 50-90 ℃, and stirring for 1-5 h;
cooling to 20-40 ℃, adding the aqueous epoxy resin and the inorganic salt into the device, and continuously stirring for 1-2 h to generate the asphalt emulsifier.
10. An asphalt comprising the asphalt emulsifier of any one of claims 6 to 8.
CN201911396460.XA 2019-12-30 2019-12-30 Lignin emulsifier, asphalt emulsifier, preparation method of asphalt emulsifier and asphalt Pending CN112521623A (en)

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Application publication date: 20210319