CN115260386B - Cationic polyacrylamide inverse emulsion, preparation method and application thereof - Google Patents
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Abstract
The invention discloses a cationic polyacrylamide inverse emulsion, a preparation method and application thereof, and belongs to the technical field of acrylamide inverse emulsion polymerization. The preparation method comprises the steps of controlling the type and the dosage of the cationic monomer before and after pH adjustment, and preparing a water phase; emulsifying, polymerizing, and adding stabilizer to obtain the cationic polyacrylamide reverse emulsion. The reverse emulsion prepared by the invention avoids the hydrolysis of the cationic monomer in the preparation process of the emulsion, and utilizes the stabilizer to maintain the pH stability of the system in the storage process, thereby further reducing the generation of hydrolysis. The inverse emulsion can be used in the field of papermaking, and can effectively solve the problem that a filter screen is easy to block due to excessive insoluble substances generated by hydrolysis in the use process of the inverse emulsion.
Description
Technical Field
The invention belongs to the technical field of acrylamide inverse emulsion polymerization, and particularly relates to a cationic polyacrylamide inverse emulsion, and a preparation method and application thereof.
Background
With the increasing living standard of people, the requirement on the living paper is increased and refined gradually, and the papermaking industry also has the characteristics of increasing direction and various advantages. The auxiliary agents in the papermaking field are divided into papermaking retention aids and papermaking filter aids according to functions: wherein, the retention aid has coagulation and flocculation functions, so that the retention aid is used for improving retention rate of fine fibers and fillers in the paper stock and reducing solid content of the fine materials in water; the filter aid is mainly capable of flocculating the fine fibers on the fiber surface, and has the effects of reducing the clogging of wet paper pores and increasing permeability. The cationic polyacrylamide reverse phase emulsion has good fluidity and high dissolution speed because the cationic groups can be combined with the hydrogen bonds of the cellulose, and is widely used and researched in the field of papermaking.
The increasing demand for paper, which depends not only on the increase of the number of production lines, but also on the increasing speed of the paper machine, requires the use of inverse emulsions as retention and drainage aids, which not only have excellent performance properties, but also have higher requirements on their hydrolysis resistance, because: after being diluted and dissolved in a mixing tank, the cationic polyacrylamide inverse emulsion passes through a plurality of filters and reaches a use production line; in a paper mill, the cleaning of a dissolving tank and a filter is a timing action, and an inverse emulsion which is easy to hydrolyze generates more insoluble substances, so that the insoluble substances on the wall of the dissolving tank are accumulated, the filter is blocked, the cleaning frequency of the dissolving tank and the filter is increased, and the production line efficiency is influenced.
The traditional inverse emulsion preparation process, particularly the water phase preparation process, usually dissolves a cationic monomer and acrylamide and the like in deionized water together, neglects the problem that the cationic monomer is easy to hydrolyze under the condition of high pH, influences the activity of the monomer and reduces the application performance of the product.
Disclosure of Invention
In order to overcome the technical defects, the invention provides a cationic polyacrylamide inverse emulsion, a preparation method and application thereof, so as to solve the problems related to the background technology.
The invention provides a cationic polyacrylamide reverse phase emulsion, a preparation method and application thereof, comprising the following steps:
step 1, adding acrylamide, a first cationic monomer, a water quality stabilizer and a molecular weight regulator into deionized water, stirring for dissolving, regulating the pH to 2.0-5.0 by using a pH regulator, and then adding a second cationic monomer to obtain a water phase;
step 3, introducing inert gas into the pre-emulsion obtained in the step 2 to remove oxygen, adding an oxidant, and dropwise adding a reducing agent to initiate polymerization, wherein the polymerization temperature is controlled at 10-110 ℃;
and 4, after the polymerization reaction in the step 3 is finished, cooling, adding a stabilizer, uniformly stirring, and discharging to obtain the cationic polyacrylamide inverse emulsion.
Preferably or alternatively, the first cationic monomer is one or more of acryloyloxyethyltrimethyl ammonium chloride, methacryloyloxyethyltrimethylammonium chloride, acryloyloxyethyldimethylbenzyl ammonium chloride;
the second cationic monomer is one or more of acryloyloxyethyl trimethyl ammonium chloride, methacryloyloxyethyl trimethyl ammonium chloride and acryloyloxyethyl dimethyl benzyl ammonium chloride;
the total dosage of the first cationic monomer and the second cationic monomer accounts for 5-50% of the total mass of the emulsion, wherein the dosage of the first cationic monomer accounts for 0-10% of the total mass of the emulsion, and the dosage of the second cationic monomer accounts for 5-40% of the total mass of the emulsion.
Preferably or alternatively, the pH adjuster is one or more of itaconic acid, adipic acid, acrylic acid, glacial acetic acid, citric acid, maleic acid, malic acid, ammonium sulfate and ammonium chloride;
the pH regulator is one or a mixture of itaconic acid, adipic acid, acrylic acid, glacial acetic acid, citric acid, maleic acid, malic acid, ammonium sulfate and ammonium chloride;
the oxidant is selected from one or more of sodium persulfate, potassium bromate, ammonium persulfate, sodium bromate, hydrogen peroxide and tert-butyl hydroperoxide;
the molecular weight regulator is one or a mixture of sodium hypophosphite, sodium formate and dodecyl mercaptan.
Preferably or optionally, the complex emulsifier is selected from one or more of Span series, tween series and polymeric emulsifiers.
Preferably or optionally, the high molecular emulsifier in the composite emulsifier is one or more of Hypermer 1031, hypermer 1083, hypermer 2234, hypermer 2296, atlas G-1086 and Atlas G-1096, and the amount of the high molecular emulsifier is 1.0-2.5% of the total mass of the emulsion.
Preferably or alternatively, the stabilizer comprises at least one material having the formula; the structural formula is as follows:
wherein R is 1 Is H, CH 3 、CH 2 -CH 2 -one of OH; r is 2 Is H, CH 3 、CH 2 -CH 2 -one of OH; r 3 Is H, CH 3 One of (1); r 4 Is H, CH 3 One of (1) and (b).
Preferably or alternatively, the stabilizer comprises one or more of triethanolamine, N-dimethylethanolammonium, 2-amino-2-methyl-propanol;
and the dosage of the stabilizer accounts for 0.001-0.5% of the total mass of the emulsion.
Preferably or alternatively, the solvent oil is one or more of dearomatized solvent oil D80, D100, D110, cyclohexane, white oil and general transformer oil;
the oxidant is one or more of sodium sulfate, potassium persulfate, potassium bromate, ammonium persulfate, sodium bromate, hydrogen peroxide and tert-butyl hydroperoxide; the dosage of the oxidant accounts for 0.001 to 0.1 percent of the total mass of the emulsion;
the reducing agent is one or more of sodium sulfite, sodium bisulfite, sodium metabisulfite, sodium thiosulfate, ferrous chloride and oxalic acid, the dosage of the reducing agent accounts for 0-0.35 percent of the total mass of the emulsion, and the mass concentration of the reducing agent solution is 0.07-0.7 percent.
In a second aspect, the invention further provides a cationic polyacrylamide inverse emulsion obtained based on the preparation method of the cationic polyacrylamide inverse emulsion.
In a second aspect, the invention also provides an application of the cationic polyacrylamide reverse phase emulsion as a retention and drainage aid in the field of papermaking.
The invention relates to a cationic polyacrylamide reverse phase emulsion, a preparation method and application thereof, compared with the prior art, the cationic polyacrylamide reverse phase emulsion has the following beneficial effects: on one hand, the method optimizes the adding sequence and the corresponding proportion of the cationic monomers, can reduce the hydrolysis of ester bonds of the cationic monomers to the minimum degree under high pH, and can ensure the activity of the cationic monomers when reacting with acrylamide by adding the cationic monomers when the pH is 2-5 and keeping the ester bonds in the cationic monomers in a stable state;
on the other hand, hydrolysis of acrylamide after polymerization is inevitable, hydrolysis products are mainly acrylic acid, carboxyl of the acrylic acid has an accelerating effect on hydrolysis of ortho-amido, and the invention neutralizes the acrylic acid by adding the stabilizing agent, thereby eliminating the influence of the carboxyl on the ortho-amido, maintaining the relative stability of the pH of the system and reducing the condition that the acrylamide copolymer accelerates hydrolysis due to the increase of the hydrolysis degree. The two are combined, so that the problem that the filter screen is easy to block due to excessive insoluble substances generated by hydrolysis is solved to the maximum extent.
Drawings
FIG. 1 is a graph showing the viscosity change with time of cationic polyacrylamide inverse emulsions prepared in each example of the present invention and comparative example.
Fig. 2 is an actual photograph of the filter after the same time period as the actual use of example 1 and comparative example 1 according to the present invention.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present invention. It will be apparent, however, to one skilled in the art, that the present invention may be practiced without one or more of these specific details. In other instances, well-known features have not been described in order to avoid obscuring the invention.
The invention will now be further described with reference to the following examples, which are intended to be illustrative of the invention and are not to be construed as limiting the invention.
Example 1
The cationic polyacrylamide inverse emulsion is prepared by the following steps of:
(1) Preparing a water phase, wherein the water phase comprises the following components in parts by mass: weighing 3 parts of acrylamide and 0.02 part of diethylenetriamine pentaacetic acid pentasodium salt, adding the weighed acrylamide and the 0.02 part of diethylenetriamine pentaacetic acid pentasodium salt into 30 parts of deionized water, stirring and dissolving, adjusting the pH value to 2.8, adding 40 parts of acryloyloxyethyl trimethyl ammonium chloride (DAC), and stirring and dissolving to obtain a water phase;
(2) Preparing and emulsifying an oil phase: dissolving 2 parts of Span60, 2.5 parts of Tween80 and 1.2 parts of Hypermer 2234 in 20 parts of dearomatized solvent oil D80, and uniformly stirring to obtain an oil phase; then, dropwise adding the water phase obtained in the step (1) into the oil phase, and stirring and emulsifying for 40min to obtain a pre-emulsion;
(3) Polymerization reaction: introducing inert gas into the pre-emulsion obtained in the step (2) to remove oxygen, adding 0.008 part of potassium persulfate, and dropwise adding 0.05 part (mass concentration is 0.38%) of sodium bisulfite to initiate polymerization, wherein the polymerization temperature is controlled to be 20-80 ℃, and the initiation time is 1.5 hours;
(4) And (3) post-treatment: and (4) after the polymerization reaction in the step (3) is finished, cooling to 30 ℃, adding 0.3 part of triethanolamine, uniformly stirring, and discharging to obtain the cationic polyacrylamide inverse emulsion.
Example 2
The cationic polyacrylamide inverse emulsion is prepared by the following steps of:
(1) Preparing a water phase, wherein the water phase comprises the following components in parts by mass: weighing 4 parts of acrylamide, 1 part of acryloyloxyethyl dimethyl benzyl ammonium chloride (DABC) and 0.01 part of ethylene diamine tetraacetic acid sodium salt, adding the materials into 31 parts of deionized water, stirring and dissolving, adjusting the pH value to 2.1, adding 35 parts of acryloyloxyethyl trimethyl ammonium chloride (DAC), and stirring and dissolving to obtain a water phase;
(2) Preparing and emulsifying an oil phase: dissolving 1.9 parts of Span60, 1.8 parts of Tween80 and 2 parts of Hypermer 1083 in 22 parts of white oil, and uniformly stirring to obtain an oil phase; then, dropwise adding the water phase obtained in the step (1) into the oil phase, and stirring and emulsifying for 30min to obtain a pre-emulsion;
(3) Polymerization reaction: introducing inert gas into the pre-emulsion obtained in the step (2) to remove oxygen, adding 0.008 part of ammonium persulfate, dropwise adding 0.1 part (mass concentration is 0.45%) of sodium bisulfite to initiate polymerization, controlling the polymerization temperature at 20-90 ℃ and initiating for 1 hour;
(4) And (3) post-treatment: and (4) after the polymerization reaction in the step (3) is finished, cooling to 40 ℃, adding 0.1 part of N, N-dimethylethanolamine, uniformly stirring, and discharging to obtain the cationic polyacrylamide inverse emulsion.
Example 3
The cationic polyacrylamide inverse emulsion is prepared by the following steps of:
(1) Preparing a water phase, wherein the mass portions are as follows: weighing 10 parts of acrylamide, 7 parts of acryloyloxyethyl trimethyl ammonium chloride (DAC) and 0.015 part of diethylenetriamine pentaacetic acid pentasodium salt, adding into 35 parts of deionized water, stirring and dissolving, adjusting the pH value to 3.3, adding 25 parts of dimethyl diallyl ammonium chloride (DADMAC), and stirring and dissolving to obtain a water phase;
(2) Preparing and emulsifying an oil phase: dissolving 2.4 parts of Span60, 1.7 parts of Tween81 and 1.6 parts of Atlas G-1086 in 16 parts of dearomatized solvent oil D110, and uniformly stirring to obtain an oil phase; then, dropwise adding the water phase obtained in the step (1) into the oil phase, and stirring and emulsifying for 60min to obtain a pre-emulsion;
(3) Polymerization reaction: introducing inert gas into the pre-emulsion obtained in the step (2) to remove oxygen, adding 0.003 part of potassium persulfate, and dropwise adding 0.15 part (mass concentration is 0.3%) of sodium thiosulfate to initiate polymerization, wherein the polymerization temperature is controlled to be 20-90 ℃, and the initiation time is 1.5 hours;
(4) And (3) post-treatment: and (4) after the polymerization reaction in the step (3) is finished, cooling to 40 ℃, adding 0.02 part of N, N-dimethylethanolamine, uniformly stirring, and discharging to obtain the cationic polyacrylamide inverse emulsion.
Example 4
This example prepares a cationic polyacrylamide inverse emulsion by the following steps:
(1) Preparing a water phase, wherein the mass portions are as follows: weighing 20 parts of acrylamide, 3 parts of acryloyloxyethyltrimethyl ammonium chloride (DAC) and 0.01 part of ethylene diamine tetraacetic acid sodium salt, adding into 27 parts of deionized water, stirring for dissolving, adjusting the pH value to 3.6, adding 20 parts of acryloyloxyethyltrimethyl ammonium chloride (DAC), and stirring for dissolving to obtain a water phase;
(2) Preparing and emulsifying an oil phase: dissolving 2 parts of Span80, 1.2 parts of Tween81 and 2.5 parts of Hypermer 1083 in 23 parts of universal transformer oil, and uniformly stirring to obtain an oil phase; then, dropwise adding the water phase obtained in the step (1) into the oil phase, and stirring and emulsifying for 60min to obtain a pre-emulsion;
(3) Polymerization reaction: introducing inert gas into the pre-emulsion obtained in the step (2) to remove oxygen, adding 0.003 part of ammonium persulfate, and dropwise adding 0.25 part (mass concentration is 0.25%) of sodium thiosulfate to initiate polymerization, wherein the polymerization temperature is controlled to be 17-100 ℃, and the initiation time is 1.5 hours;
(4) And (3) post-treatment: after the polymerization reaction in the step (3) is finished, cooling to 30 ℃, adding 0.2 part of triethanolamine and N, N-dimethylethanolamine (the mass ratio is 1:3-3:1), uniformly stirring, and discharging to obtain the cationic polyacrylamide inverse emulsion.
Example 5
The cationic polyacrylamide inverse emulsion is prepared by the following steps of:
(1) Preparing a water phase, wherein the water phase comprises the following components in parts by mass: weighing 24 parts of acrylamide, 4 parts of methacryloyloxyethyl trimethyl ammonium chloride (DMC) and 0.018 part of diethylenetriamine pentaacetic acid pentasodium salt, adding into 36 parts of deionized water, stirring and dissolving, adjusting the pH value to 2.5, adding 11 parts of methacryloyloxyethyl trimethyl ammonium chloride (DMC), stirring and dissolving to obtain a water phase;
(2) Preparing and emulsifying an oil phase: dissolving 1.5 parts of Span60, 2 parts of Tween85 and 2 parts of Hypermer 2296 in 19 parts of dearomatized solvent oil D100, and uniformly stirring to obtain an oil phase; then, dropwise adding the water phase obtained in the step (1) into the oil phase, and stirring and emulsifying for 30min to obtain a pre-emulsion;
(3) Polymerization reaction: introducing inert gas into the pre-emulsion obtained in the step (2) to remove oxygen, adding 0.005 part of sodium persulfate, dropwise adding 0.2 part (mass concentration is 0.2%) of sodium metabisulfite to initiate polymerization, controlling the polymerization temperature to be 13-105 ℃, and initiating for 2 hours;
(4) And (3) post-treatment: and (4) after the polymerization reaction in the step (3) is finished, cooling to 35 ℃, adding 0.21 part of N, N-dimethylethanolamine, uniformly stirring, and discharging to obtain the cationic polyacrylamide inverse emulsion.
Example 6
The cationic polyacrylamide inverse emulsion is prepared by the following steps of:
(1) Preparing a water phase, wherein the mass portions are as follows: weighing 32 parts of acrylamide, 5 parts of methacryloxyethyl trimethyl ammonium chloride (DMC) and 0.015 part of ethylene diamine tetraacetic acid sodium salt, adding into 34 parts of deionized water, stirring and dissolving, adjusting the pH value to 4.5, adding 5 parts of methacryloxyethyl trimethyl ammonium chloride (DMC), stirring and dissolving to obtain a water phase;
(2) Preparing and emulsifying an oil phase: dissolving 1.8 parts of Span80, 2.9 parts of Tween61 and 1 part of Atlas G-1096 in 17 parts of cyclohexane, and uniformly stirring to obtain an oil phase; then, dropwise adding the water phase obtained in the step (1) into the oil phase, and stirring and emulsifying for 30min to obtain a pre-emulsion;
(3) Polymerization reaction: introducing inert gas into the pre-emulsion obtained in the step (2) to remove oxygen, adding 0.009 part of tert-butyl hydroperoxide, dropwise adding 0.35 part (mass concentration is 0.25%) of sodium metabisulfite to initiate polymerization, controlling the polymerization temperature at 15-105 ℃ and initiating for 1 hour;
(4) And (3) post-treatment: after the polymerization reaction in the step (3) is finished, cooling to 35 ℃, adding 0.015 part of N, N-dimethylethanolamine and 2-amino-2-methyl-propanol (the mass ratio is 1:1-5:1), uniformly stirring, and discharging to obtain the cationic polyacrylamide inverse emulsion.
Comparative example 1
This comparative example is compared with the production method in example 1, and the polymerization process in step (1) and step (4) in this comparative example is different from that in example 1, and the production method in this comparative example has the following steps:
the preparation process of example 1 was followed, adjusting step (1) to:
preparing a water phase, wherein the water phase comprises the following components in parts by mass: weighing 3 parts of acrylamide, 35 parts of acryloyloxyethyl trimethyl ammonium chloride (DAC) and 0.02 part of diethylenetriamine pentaacetic acid pentasodium salt, adding the weighed materials into 30 parts of deionized water, stirring and dissolving, adjusting the pH value to 2.8, adding 5 parts of acryloyloxyethyl trimethyl ammonium chloride (DAC) and 0.008 part of potassium persulfate, and stirring and dissolving to obtain a water phase;
the preparation method of example 1 was followed in step (2) and step (3), without adjustment;
the preparation process of example 1 was followed, adjusting step (4) to:
and (3) post-treatment: and (4) after the polymerization reaction in the step (3) is finished, cooling to 30 ℃, and discharging to obtain the cationic polyacrylamide inverse emulsion.
Detection and discussion
The cationic polyacrylamide inverse emulsions obtained in examples and comparative examples were dissolved in tap water at a concentration of 0.6wt% for 1 hour with stirring, and the samples dissolved in examples 1 to 6 and comparative examples were designated as samples 1 to 7 in this order. The viscosity change is tested at room temperature within 24 hours; the results are shown in FIG. 1, where samples 1-6 all had a viscosity reduction of < 50% and sample 7 had a viscosity reduction of > 90%.
When the inverse emulsion prepared by the preparation method of comparative example 1 is used in a paper mill, the cleaning frequency of a dissolving tank and a filter is 2 times that of example 1, which has a considerable influence on the stable production of a production line, and the filter conditions of example 1 and comparative example 1 are shown in fig. 2.
It should be noted that the various features described in the foregoing embodiments may be combined in any suitable manner without contradiction. The invention is not described in detail in order to avoid unnecessary repetition.
Claims (11)
1. The preparation method of the cationic polyacrylamide inverse emulsion is characterized by comprising the following steps:
step 1, adding acrylamide, a first cationic monomer, a water quality stabilizer and a molecular weight regulator into deionized water, stirring for dissolving, regulating the pH to 2.0-5.0 by using a pH regulator, and then adding a second cationic monomer to obtain a water phase;
step 2, dissolving the composite emulsifier in the solvent oil, and uniformly stirring to obtain an oil phase; then, dropwise adding the water phase obtained in the step 1 into the oil phase, and stirring to obtain a pre-emulsion;
3, introducing inert gas into the pre-emulsion obtained in the step 2 to remove oxygen, adding an oxidant, and dropwise adding a reducing agent to initiate polymerization, wherein the polymerization temperature is controlled at 10-110 ℃;
after the polymerization reaction in the step 4 and the step 3 is finished, cooling, adding a stabilizer, uniformly stirring, and discharging to obtain a cationic polyacrylamide inverse emulsion;
the first cationic monomer is one or more of acryloyloxyethyl trimethyl ammonium chloride, methacryloyloxyethyl trimethyl ammonium chloride and acryloyloxyethyl dimethyl benzyl ammonium chloride;
the second cationic monomer is one or more of acryloyloxyethyltrimethyl ammonium chloride, methacryloyloxyethyltrimethylammonium chloride and acryloyloxyethyldimethylbenzyl ammonium chloride;
the total dosage of the first cationic monomer and the second cationic monomer accounts for 5-50% of the total mass of the emulsion, wherein the dosage of the first cationic monomer accounts for 0-10% of the total mass of the emulsion, and the dosage of the second cationic monomer accounts for 5-40% of the total mass of the emulsion;
the stabilizer at least comprises a substance with the following structural formula; the structural formula is as follows:
wherein R is 1 Is H, CH 3 、CH 2 -CH 2 -one of OH; r 2 Is H, CH 3 、CH 2 -CH 2 -one of OH; r 3 Is H, CH 3 One kind of (1); r 4 Is H, CH 3 One of (1) and (b).
2. The method for preparing the cationic polyacrylamide inverse emulsion according to claim 1, wherein the pH regulator is one or more of itaconic acid, adipic acid, acrylic acid, glacial acetic acid, citric acid, maleic acid and malic acid.
3. The method for preparing the cationic polyacrylamide reverse phase emulsion according to claim 1, wherein the molecular weight regulator is one or more of sodium hypophosphite, sodium formate and dodecyl mercaptan.
4. The method for preparing the cationic polyacrylamide reverse phase emulsion according to claim 1, wherein the composite emulsifier is selected from one or more of Span series, tween series and high molecular emulsifiers.
5. The method for preparing the cationic polyacrylamide reverse phase emulsion according to claim 4, wherein the high molecular weight emulsifier in the composite emulsifier is one or more of Hypermer 1031, hypermer 1083, hypermer 2234, hypermer 2296, atlas G-1086 and Atlas G-1096, and the amount of the high molecular weight emulsifier is 1.0-2.5% of the total mass of the emulsion.
6. The method of claim 1, wherein the stabilizer comprises one or more of triethanolamine, N-dimethylethanolammonium, 2-amino-2-methyl-propanol;
and the dosage of the stabilizer accounts for 0.001-0.5% of the total mass of the emulsion.
7. The method for preparing the cationic polyacrylamide inverse emulsion according to claim 1, wherein the solvent oil is one or more of dearomatized solvent oils D80, D100, D110, cyclohexane, white oil and general transformer oil.
8. The method for preparing the cationic polyacrylamide inverse emulsion according to claim 1, wherein the oxidant is one or more of sodium persulfate, potassium bromate, ammonium persulfate, sodium bromate, hydrogen peroxide and tert-butyl hydroperoxide; the dosage of the oxidant accounts for 0.001-0.1% of the total mass of the emulsion.
9. The method for preparing the cationic polyacrylamide inverse emulsion according to claim 1, wherein the reducing agent is one or more of sodium sulfite, sodium bisulfite, sodium metabisulfite, sodium thiosulfate, ferrous chloride and oxalic acid, the amount of the reducing agent is 0-0.35% of the total mass of the emulsion, and the mass concentration of the reducing agent solution is 0.07-0.7%.
10. A cationic polyacrylamide inverse emulsion obtained by the method for preparing a cationic polyacrylamide inverse emulsion according to any one of claims 1 to 9.
11. Use of the cationic polyacrylamide inverse emulsion according to claim 10 as a retention and drainage aid in the papermaking field.
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