CN115677924B - Low molecular weight polyacrylamide colloidal particle and preparation method thereof - Google Patents
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Abstract
The application discloses a low molecular weight polyacrylamide colloidal particle and a preparation method thereof, and belongs to the technical field of water-soluble polyacrylamide. The polyacrylamide colloid with the molecular weight smaller than 100w is prepared through oxidation-reduction reaction, and in order to prevent the low-molecular-weight polyacrylamide colloid from being softer and more viscous after the concentration of the low-molecular-weight polyacrylamide colloid exceeds 50 percent, a colloid reinforcing agent consisting of a reactive cross-linking agent, a non-reactive micromolecule and a non-reactive polar oligomer is added into a polymerization system. The low molecular weight polyacrylamide colloidal particles avoid insoluble substances caused by overhigh temperature in the fluidized bed drying process, greatly reduce energy loss in the drying process, can be applied to paper fiber modification, and have simple and continuous preparation method and process, high efficiency and high yield.
Description
Technical Field
The application relates to the technical field of water-soluble polyacrylamide, in particular to a low molecular weight polyacrylamide colloidal particle and a preparation method thereof.
Background
Polyacrylamide is a common name of acrylamide homopolymer or a polymer obtained by copolymerizing acrylamide homopolymer with other monomers, and is one of the most widely used varieties of water-soluble polymers. As the polyacrylamide structural unit contains amide groups, is easy to form hydrogen bonds, has good water solubility and high chemical activity, is easy to obtain various modified matters with branched chains or net structures through grafting or crosslinking, and is widely applied to industries such as petroleum exploitation, water treatment, textile, papermaking, mineral separation, medicine, agriculture and the like.
The polyacrylamide products are various and mainly comprise solid, liquid and emulsion, and in the papermaking industry, the effect of modifying paper fibers can be achieved by improving the distribution, the binding capacity and the retention of paper pulp fibers. However, the existing polyacrylamide products for improving the paper strength mainly comprise aqueous solution products, and have the advantages of low content, high transportation cost, long production period, difficulty in realizing continuous production, short quality guarantee period and easiness in influence of environmental factors on product quality to cause product deterioration or index fluctuation. The low molecular weight solid polyacrylamide colloid has high soft viscosity, and is easy to cause excessive physical extrusion during processing and granulation, thereby causing the adverse effects of increased insoluble substances and the like; when the fluidized bed is dried, the phenomenon that insoluble substances are increased due to crosslinking is easy to occur at the drying temperature of more than 85 ℃.
Therefore, there is a need for a low molecular weight polyacrylamide gel particle that is simple in preparation process, high in yield, economical in production cost, and less prone to binding.
Disclosure of Invention
In order to solve the existing technical problems, 1. A preparation method of low molecular weight polyacrylamide colloidal particles is characterized by comprising the following steps:
preparing a monomer aqueous solution: uniformly mixing deionized water, ionic monomer, solid acrylamide, chain transfer agent, chelating agent, colloid reinforcing agent and acid-base buffer to form polymerization solution; the polymerization liquid comprises the following components in percentage by mass: 56-59% of acrylamide, 10-20% of ionic monomer, 0.005-0.02% of chain transfer agent, 0.008-0.04% of chelating agent, 0.8-0.9% of colloid reinforcing agent and the balance of deionized water;
and (3) polymerizing to prepare colloidal particles: controlling the height of the polymerization liquid, regulating the pH value, adding an oxidant, a reducing agent and an azo initiator into the polymerization liquid, heating to 55-65 ℃, reacting for 5-10min, then, increasing the reaction temperature to 120-140 ℃, naturally cooling for 10-20min, granulating for the first time before the colloid is hardened, and preparing the polymer colloid after the reaction is finished, wherein the particle size is 3-5mm;
and (3) cooling and granulating: and crushing, drying and cooling the cooled colloid, and grinding and screening to obtain the paper fiber modifier colloidal particles.
Preferably or alternatively, the height of the polymerization liquid is controlled to be 3-4cm, and the pH value is adjusted to be 2.5-4.5.
Preferably or alternatively, the colloidal reinforcing agent includes a reactive cross-linking agent, a non-reactive small molecule compound, and a non-reactive polar oligomer.
Preferably or alternatively, the reactive cross-linking agent comprises N, N-methylenebisacrylamide, N-methylolacrylamide, polyallylamine; the non-reactive small molecular compound comprises urea, sodium chloride, ammonium sulfate, acetamide, ammonium adipate and ammonium chloride; the non-reactive polar oligomer comprises polyethylene oxide, polyvinyl alcohol and polyamine with molecular weight less than 10000.
Preferably or alternatively, the azo initiator is used in an amount of 0.03-0.05% of the mass of the acrylamide and the ionic monomer, the oxidant is used in an amount of 0.5-0.8% of the mass of the acrylamide and the ionic monomer, and the reducing agent is 80-120% of the oxidant.
Preferably or alternatively, the chelating agent comprises EDTA-2Na, DTPA-5Na; the buffering agent comprises hydrochloric acid, sulfuric acid, acetic acid, phosphoric acid, nitric acid, citric acid, formic acid, acetic acid, propionic acid, adipic acid, benzoic acid, sodium hydroxide, potassium hydroxide and sodium carbonate; the chain transfer agent includes lower aliphatic alcohols, polyethylene glycols, benzyl alcohols, hypophosphites, formates, alkyl sulfonates, (meth) allyl sulfonates, mercaptoethanol, or alkyl mercaptans.
Preferably or alternatively, the oxidant solution comprises 5% by mass of ammonium persulfate, sodium persulfate, potassium persulfate, hydrogen peroxide, tert-butyl hydroperoxide, benzoyl peroxide, sodium bromate, potassium bromate; the reducer solution comprises sodium bisulphite, sodium sulfite, sodium metabisulfite, sodium dithionite, ferrous sulfate, ferrous ammonium sulfate, triethylamine, triethanolamine and tetramethyl ethylenediamine with mass percent of 5%.
A low molecular weight polyacrylamide gel particle obtained based on the preparation method of any one of the above-mentioned low molecular weight polyacrylamide gel particles, characterized in that the solid content of the low molecular weight polyacrylamide gel particle is not less than 80%.
The beneficial effects are that: the application provides a low molecular weight polyacrylamide colloidal particle and a preparation method thereof, wherein the polyacrylamide colloidal particle with the molecular weight smaller than 100w is prepared through oxidation-reduction reaction, and in order to prevent the characteristic that the low molecular weight polyacrylamide colloidal particle still presents softer texture and high viscosity after the concentration exceeds 50 percent, the solid acrylamide is directly used for participating in polymerization reaction, a colloid reinforcing agent consisting of a reactive cross-linking agent, a non-reactive micromolecule and a non-reactive polar oligomer is added into a polymerization system, and the reactive cross-linking agent can form a net-shaped, branched and other structures, so that the density of physical entanglement points among molecular chains is improved, and the integral strength of the polyacrylamide colloidal particle is improved; the non-reactive small molecular compound can improve the hardness of the polyacrylamide colloid and the solubility of the product while improving the solid content of the product; the non-reactive polar oligomer can promote the overall hydrogen bond quantity of the polyacrylamide colloid, the number of the hydrogen bond bonding points is increased, the internal stress of the colloid is larger than the bonding force of the colloid and equipment, and the colloid is convenient to separate from the equipment, so that the strength of the colloid is improved, and the viscosity is reduced. Compared with the existing method for preparing the high-concentration polyacrylamide colloid, the method adopts a mode of combining single-stage polymerization rather than redox initiation and ultraviolet initiation, and the prepared polymerization product is the polyacrylamide colloid with extremely high solid content, rather than the polyacrylamide colloid solution with the mass concentration lower than 60 percent, and the polymerization temperature is as high as 130 ℃, so that the polymerization heat is not required to be removed in the reaction process. The prepared high-solid-content rubber particles avoid insoluble substances caused by overhigh temperature in the fluidized bed drying process, and simultaneously greatly reduce energy loss in the drying process.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present application. It will be apparent, however, to one skilled in the art that the application may be practiced without one or more of these details. In other instances, well-known features have not been described in detail in order to avoid obscuring the application.
The application is further illustrated below in conjunction with examples, examples of which are intended to illustrate the application and are not to be construed as limiting the application. The specific techniques and reaction conditions not specified in the examples may be carried out according to the techniques or conditions described in the literature in this field or the product specifications. Reagents, instruments or equipment not specifically mentioned in the manufacturer are commercially available.
The preparation method of the low molecular weight polyacrylamide colloidal particle comprises the following steps:
step one, preparing solid acrylamide and a comonomer into an aqueous solution; the solid acrylamide and the copolymerization are prepared into aqueous solution with the monomer concentration of 70-75wt%, wherein the monomer concentration is formed by combining monomers with different activities, and the content of the acrylamide in the total monomers accounts for 66-71wt%;
step two, adding a chain transfer agent, a chelating agent, a colloid reinforcing agent and an acid-base buffer into the aqueous solution prepared in the step one, and uniformly mixing to form a polymerization solution;
step three, controlling the height of the polymerization liquid to ensure that the height range of the polymerization liquid is 3-4cm; the pH value is regulated to 2.5-4.5 by sulfuric acid or sodium hydroxide; heating the polymerization solution to 55-65 ℃, and adding an oxidant solution with the mass concentration of 5-10wt% and a reducing agent solution with the mass concentration of 5-10wt% for polymerization reaction; in this embodiment, when the polymerization reaction is performed on the polymerization solution, the mass concentration of each component is as follows: 46-49wt% of acrylamide, 10-20wt% of comonomer, 0.005-0.02wt% of chain transfer agent, 0.008-0.04wt% of chelating agent, 0.8-0.9wt% of colloid reinforcing agent, 0.03-0.05wt% of azo initiator, 0.5-0.8wt% of oxidant solution and 0.5-0.8wt% of reducing agent solution. In the test, in order to better promote the polymerization reaction and the colloid cooling: too thin colloid can cause heat dissipation of polymerization reaction, and influence polymerization; the excessive thickness of the colloid can lead to large heat release of polymerization, prolong the cooling time of the colloid and is unfavorable for cutting the colloid and granulating; experiments prove that the thickness of the glue block of 3-4cm has the best effect on polymerization reaction, colloid cooling and colloid cutting granulation.
Step four, after polymerization reaction for 5-10min in the step three, polyacrylamide colloid with molecular weight below 60w is obtained; the polymerization reaction process in the embodiment is carried out in an open place with heat exchange outside, the highest temperature is 120-140 ℃, the temperature is naturally reduced for 10-20min after the highest temperature is reached, primary granulation is carried out before the colloid is hardened, and the particle size is 3-5mm;
and fifthly, placing the colloidal particles obtained in the step four in a drying environment for natural cooling, cooling to room temperature, and directly grinding and sieving to obtain products with three particle size specifications, wherein the moisture of the colloidal particles is 10-15%: > 20 mesh, 20-60 mesh, < 60 mesh.
The colloidal reinforcing agent has a wide selection range, and can be prepared by one or more of a reactive cross-linking agent, a non-reactive micromolecular compound for improving the solid content and a non-reactive polar oligomer for improving the hydrogen bond effect; the reactive cross-linking agent comprises one or more of N, N-methylenebisacrylamide, N-methylolacrylamide and polyallylamine; the small molecular compound comprises one or more of urea, sodium chloride, ammonium sulfate, acetamide, ammonium adipate and ammonium chloride; the polar oligomer comprises one or more of polyethylene oxide, polyvinyl alcohol and polyamine with molecular weight below 10000. In the preparation method of the embodiment, the polyacrylamide colloid with the molecular weight below 100w is still softer and has high viscosity even if the concentration exceeds 50%, and the defects can be well compensated by adopting the colloid reinforcing agent; the reactive cross-linking agent is added to form a net-shaped, branched and other structure, so that the physical entanglement points are increased, and the integral strength of the polyacrylamide colloid is improved; after the micromolecular compound is added, on one hand, the solid content of the product can be improved, the colloid hardness is improved, the continuous production is convenient, and on the other hand, the addition of the micromolecular compound can promote the dissolution of the product; the polar oligomer is added to promote the overall hydrogen bond number of the polyacrylamide colloid, the number of the hydrogen bond bonding points is increased, the internal stress of the colloid is larger than the bonding force of the colloid and equipment, and the colloid is convenient to separate from the equipment, so that the strength and the viscosity of the colloid are improved. And selecting a proper medicament according to the situation, and adding and deleting colloid reinforcing agent selection aiming at the product.
Example 1
According to the preparation method of the low molecular weight polyacrylamide colloidal particles, the preparation method is verified by experimental data of specific numerical values:
firstly, preparing a polymerization solution according to the content in the first to third steps, adding 5g of glacial acetic acid, 5g of anhydrous citric acid, 110g of solid acrylamide, 5.625g of 80% by mass of methacryloxyethyl trimethyl ammonium chloride, 23.55g of 60% by mass of methacryloxyethyl dimethyl benzyl ammonium chloride, 5g of dimethylaminoethyl methacrylate serving as a functional monomer, 0.1g of pentasodium ethylenediamine tetraacetate serving as a chelating agent, 2.56g of N, N-dimethylacrylamide, 0.3g of diallylamine serving as a crosslinking agent, 2g of polar oligomer PEG-8000 and 0.5g of 10% by mass of sodium hypophosphite serving as a chain transfer agent, 2g of absolute ethyl alcohol, 5g of anionic monomer itaconic acid, 7.5g of industrial refined salt for improving the colloid strength, 7.5g of cosolvent urea and 55g of deionized water into a reaction container, and stirring and dissolving uniformly;
then, after detecting the pH value of the polymerization solution to 4.0, raising the temperature of the polymerization solution to 60 ℃ by a hot water bath, adding an oxidant solution, preferably 0.8g of a 5% t-butyl hydroperoxide solution, and a reducing agent solution, preferably 0.8g of a 5% sodium metabisulfite solution, at intervals of about 30s while stirring; with the addition of the initiator, the viscosity and the temperature of the polymerization solution rise along with the rise, a large amount of water gas is released, after the reaction is carried out to the highest temperature of 132.5 ℃, the polymerization solution forms glue, and then the temperature is naturally reduced;
and after the polymerization reaction is finished, water vapor is dispersed, the colloid is cooled to about 80 ℃, the colloid is taken out, granulation is carried out in a dry environment, drying and cooling are carried out by blowing the colloidal particles with dry and cold gas, the water content of the obtained colloidal particles is 12.18%, grinding can be directly carried out, then screening is carried out by using a screen, three colloidal particles with different particle size specifications are obtained by screening, the molecular weight of the obtained colloidal particles is 55.8 ten thousand, and the insoluble content is less than 0.05ml/L.
Example 2
The preparation method and the verification method of the low molecular weight polyacrylamide gel particles in this example are the same as those in example 1.
According to the content in the first to third steps, preparing a polymerization solution, adding 5g of glacial acetic acid, 5g of anhydrous citric acid, 110g of solid acrylamide, 5.625g of 80% of methacryloyloxyethyl trimethyl ammonium chloride, 23.55g of 60% of methacryloyloxyethyl dimethyl benzyl ammonium chloride, 5g of dimethylaminoethyl methacrylate serving as a functional monomer, 0.1g of pentasodium ethylenediamine tetraacetate serving as a chelating agent, 2.56g of N, N-dimethylacrylamide, 0.3g of diallylamine serving as a crosslinking agent, 2g of polar oligomer PEG-8000 and 0.5g of 10% sodium hypophosphite serving as a chain transfer agent, 2g of absolute ethyl alcohol, 5g of anionic monomer itaconic acid, 7.5g of industrial refined salt for improving the colloid strength, 7.5g of cosolvent urea and 55g of deionized water into a reaction container, stirring and dissolving uniformly;
then, the pH of the polymerization solution is regulated to 3.0 by sulfuric acid, the polymerization solution after the pH regulation is heated to 60+/-1 ℃ by a hot water bath, an oxidant solution is added under stirring, a reducing agent solution is added at intervals of about 30 seconds, in the embodiment, the oxidant solution is preferably 0.8g of a 5% tertiary butyl hydroperoxide solution, and the reducing agent solution is preferably 0.8g of a 5% sodium metabisulfite solution; with the addition of the initiator, the viscosity and the temperature of the polymerization solution rise along with the rise, a large amount of water gas is released, after the reaction is carried out to the highest temperature of 132.5 ℃, the polymerization solution forms glue, and then the temperature is naturally reduced;
and after the polymerization reaction is finished, water vapor is dispersed, the colloid is cooled to about 100 ℃, the colloid is taken out, granulation is carried out in a dry environment, drying and cooling are carried out by blowing the colloidal particles with dry and cold gas, the water content of the obtained colloidal particles is 9.88%, grinding can be directly carried out, then screening is carried out by using a screen, three colloidal particles with different particle size specifications are obtained by screening, the molecular weight of the obtained colloidal particles is 52.8 ten thousand, and the insoluble content is less than 0.05ml/L.
Example 3
The preparation method and the verification method of the low molecular weight polyacrylamide gel particles in this example are the same as those in example 1.
According to the content in the first to third steps, preparing a polymerization solution, adding 5g of glacial acetic acid, 5g of anhydrous citric acid, 110g of solid acrylamide, 5.625g of 80% of methacryloyloxyethyl trimethyl ammonium chloride, 23.55g of 60% of methacryloyloxyethyl dimethyl benzyl ammonium chloride, 5g of dimethylaminoethyl methacrylate serving as a functional monomer, 0.1g of pentasodium ethylenediamine tetraacetate serving as a chelating agent, 2.56g of N, N-dimethylacrylamide, 0.3g of diallylamine serving as a crosslinking agent, 2g of polar oligomer PEG-8000 and 0.5g of 10% sodium hypophosphite serving as a chain transfer agent, 2g of absolute ethyl alcohol, 5g of anionic monomer itaconic acid, 7.5g of industrial refined salt for improving the colloid strength, 7.5g of cosolvent urea and 40g of deionized water into a reaction container, stirring and dissolving uniformly;
then, detecting the pH value of the polymerization solution to be 4.0, heating the polymerization solution to 60 ℃ through a hot water bath, adding an oxidant solution, preferably 0.8g of 5% t-butyl hydroperoxide solution, and a reducing agent solution, preferably 0.8g of 5% sodium metabisulfite solution, at intervals of about 30s under stirring; with the addition of the initiator, the viscosity and the temperature of the polymerization solution rise along with the rise, a large amount of water gas is released, and after the reaction is carried out to the highest temperature of 136.5 ℃, the polymerization solution forms glue, and then the temperature is naturally reduced;
after the polymerization reaction is finished, water vapor is dispersed, the colloid is cooled to about 80 ℃, the colloid is taken out, granulation is carried out in a dry environment, drying and cooling are carried out by blowing the colloidal particles with dry and cold gas, the water content of the obtained colloidal particles is 11.78%, grinding can be directly carried out, then screening is carried out by a screen, three colloidal particles with different particle size specifications are obtained by screening, the molecular weight of the obtained colloidal particles is 54.3 ten thousand, and the insoluble content is less than 0.05ml/L.
Example 4
The preparation method and the verification method of the low molecular weight polyacrylamide gel particles in this example are the same as those in example 1.
According to the content in the first to third steps, preparing a polymerization solution, adding 5g of glacial acetic acid, 5g of anhydrous citric acid, 110g of solid acrylamide, 5.625g of 80% of methacryloyloxyethyl trimethyl ammonium chloride, 23.55g of 60% of methacryloyloxyethyl dimethyl benzyl ammonium chloride, 5g of dimethylaminoethyl methacrylate serving as a functional monomer, 0.1g of pentasodium ethylenediamine tetraacetate serving as a chelating agent, 2.56g of N, N-dimethylacrylamide, 0.3g of diallylamine serving as a crosslinking agent, 2g of polar oligomer PEG-8000 and 0.5g of 10% sodium hypophosphite serving as a chain transfer agent, 2g of absolute ethyl alcohol, 5g of anionic monomer itaconic acid, 7.5g of industrial refined salt for improving the colloid strength, 7.5g of cosolvent urea and 40g of deionized water into a reaction container, stirring and dissolving uniformly;
then, the pH of the polymerization solution is regulated to 3.0 by sulfuric acid, the polymerization solution after the pH regulation is heated to 60+/-1 ℃ by a hot water bath, an oxidant solution is added under stirring, a reducing agent solution is added at intervals of about 30 seconds, in the embodiment, the oxidant solution is preferably 0.8g of a 5% tertiary butyl hydroperoxide solution, and the reducing agent solution is preferably 0.8g of a 5% sodium metabisulfite solution; with the addition of the initiator, the viscosity and the temperature of the polymerization solution rise along with the rise, a large amount of water gas is released, and after the reaction is carried out to the highest temperature of 136.2 ℃, the polymerization solution forms glue, and then the temperature is naturally reduced;
after the polymerization reaction is finished, water vapor is dispersed, the colloid is cooled to about 100 ℃, the colloid is taken out, granulation is carried out in a dry environment, drying and cooling are carried out by blowing the colloidal particles with dry and cold gas, the water content of the obtained colloidal particles is 9.58%, grinding can be directly carried out, then screening is carried out by a screen, three colloidal particles with different particle size specifications are obtained by screening, the molecular weight of the obtained colloidal particles is 48.88 ten thousand, and the insoluble content is less than 0.05ml/L.
Comparative example 1
The preparation method and the verification method of the low molecular weight polyacrylamide gel particles of the comparative example are the same as those of example 1. The polymerization product is dried and cooled in a fluidized bed.
Comparative example 2
The preparation method and the verification method of the low molecular weight polyacrylamide gel particles of the comparative example are the same as those of example 2. The polymerization product is dried and cooled in a fluidized bed.
Comparative example 3
The preparation method and the verification method of the low molecular weight polyacrylamide gel particles of the comparative example are the same as those of example 3. The polymerization product is dried and cooled in a fluidized bed.
Comparative example 4
The preparation method and the verification method of the low molecular weight polyacrylamide gel particles of the comparative example are the same as those of example 4. The polymerization product is dried and cooled in a fluidized bed.
Comparative example 5
238.3g of acrylamide solution with the mass fraction of 50%, 30.8g of acryloyloxyethyl trimethyl ammonium chloride with the mass fraction of 80%, 12.6g of dimethylaminopropyl methacrylamide, 0.2g of chain transfer agent sodium formate, 3g of polar oligomer PEG-800,0.1g of chelating agent ethylene diamine tetraacetic acid pentasodium and 5g of deionized water are added into a reaction kettle, and stirred and dissolved uniformly; adding a photoinitiator and an azo initiator into a reaction kettle, wherein the photoinitiator is preferably 0.15g of 1wt% Darocur1173 solution, namely 2-hydroxy-2-methyl-1-phenyl-1-acetone, the azo initiator is preferably 0.2g of 1wt% VA-044 solution, namely azo diiso Ding Mi hydrochloride, and 0.1g of 1wt% V-50 solution, namely azo diisobutylamidine dihydrochloride, stirring and mixing uniformly, and then regulating the pH value of the polymerization solution to 4.5 by sulfuric acid; then, controlling the temperature of the polymerization solution after regulating the pH value to 10 ℃ through a water bath, starting to introduce nitrogen for deoxidization, adding an oxidant solution after introducing nitrogen for 20min, and adding a reducing agent solution after continuing to introduce nitrogen for 2min, wherein the oxidant solution is preferably 6g of 10wt% tertiary butyl hydroperoxide solution, and the reducing agent solution is preferably 6g of 10wt% sodium bisulfite solution; stopping introducing nitrogen after the polymerization liquid is sticky, standing for 1h to perform a prepolymerization reaction, wherein the highest temperature in the prepolymerization reaction process is 84.3 ℃, naturally cooling after the highest temperature reaches 84.3 ℃, and then placing the reaction kettle under ultraviolet light to irradiate for 1h. Finally, the polymerization product is dried and cooled in a fluidized bed manner.
Performance comparison:
the molecular weight and insoluble content of the polyacrylamide gel particles prepared in examples 1 to 4 and comparative examples 1 to 4 are shown in the following table.
Watch (watch)
According to the table, the molecular weight of the polyacrylamide colloidal particles prepared in the examples 1-4 is lower than 60w, wherein the content of insoluble substances in each liter of colloidal particles after grinding and sieving is lower than 0.05mL. The polyacrylamide gel particles prepared in comparative examples 1-4 have extremely dispersed molecular weights, the products of comparative examples 1 and 2 are almost insoluble, the insoluble content of the products of comparative examples 3 and 4 is far greater than that of each example, and the polyacrylamide gel with the polymer concentration of 50wt% is prepared in a segmented initiation polymerization mode combining redox initiation and ultraviolet initiation, but the polymerization temperature is lower, a large amount of reaction heat is required to be removed to prevent the product from being excessively soft, so that the molecular weight of the product is lower, the solid content of the product is only 50%, and the polymerized product still needs to be dried in a fluidized bed mode, so that the insoluble content is about 6mL/L.
As described above, although the present application has been shown and described with reference to certain preferred embodiments, it is not to be construed as limiting the application itself. Various changes in form and details may be made therein without departing from the spirit and scope of the application as defined by the appended claims. The individual technical features described in the above embodiments may be combined in any suitable manner without contradiction. The various possible combinations of the application are not described in detail in order to avoid unnecessary repetition.
Claims (2)
1. The preparation method of the low molecular weight polyacrylamide colloidal particle is characterized by comprising the following steps of:
5g of glacial acetic acid, 5g of anhydrous citric acid, 110g of solid acrylamide, 5.625g of 80% of methacryloyloxyethyl trimethyl ammonium chloride, 23.55g of 60% of methacryloyloxyethyl dimethyl benzyl ammonium chloride, 5g of dimethylaminoethyl methacrylate serving as a functional monomer, 0.1g of pentasodium ethylenediamine tetraacetate serving as a chelating agent, 2.56g of N, N-dimethylacrylamide, 0.3g of diallylamine serving as a crosslinking agent, 2g of polar oligomer PEG-8000, 0.5g of 10% sodium hypophosphite serving as a chain transfer agent, 2g of absolute ethyl alcohol, 5g of anionic monomer itaconic acid, 7.5g of industrial refined salt, 7.5g of cosolvent urea and 40g of deionized water are added into a reaction vessel, and stirred and dissolved uniformly;
adjusting the pH value of the polymerization solution to 3.0 by sulfuric acid, heating the polymerization solution with the pH value adjusted to 60+/-1 ℃ by a hot water bath, adding 0.8g of 5% tertiary butyl hydroperoxide oxidant solution under stirring, and adding 0.8g of 5% sodium metabisulfite reducer solution at intervals of 30 seconds;
and after the polymerization reaction is finished, cooling the colloid to 100 ℃, taking out the colloid, granulating in a dry environment, blowing the colloid particles with dry and cold gas, drying and cooling, directly grinding, and sieving with a screen to obtain the low molecular weight polyacrylamide colloid particles.
2. The method for preparing low molecular weight polyacrylamide gel particles according to claim 1, wherein the height of the polymerization solution is controlled to be 3-4 cm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101921365A (en) * | 2010-09-09 | 2010-12-22 | 广东省工程技术研究所 | Preparation method for instant cationic polyacrylamide |
| CN109232812A (en) * | 2018-06-28 | 2019-01-18 | 江苏富淼科技股份有限公司 | A kind of cross-linking modified type water-soluble solid polyacrylamide and application thereof |
| CN112592429A (en) * | 2020-12-14 | 2021-04-02 | 江苏富淼科技股份有限公司 | Preparation method of high-concentration polyacrylamide colloid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101921365A (en) * | 2010-09-09 | 2010-12-22 | 广东省工程技术研究所 | Preparation method for instant cationic polyacrylamide |
| CN109232812A (en) * | 2018-06-28 | 2019-01-18 | 江苏富淼科技股份有限公司 | A kind of cross-linking modified type water-soluble solid polyacrylamide and application thereof |
| CN112592429A (en) * | 2020-12-14 | 2021-04-02 | 江苏富淼科技股份有限公司 | Preparation method of high-concentration polyacrylamide colloid |
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