CN111909296A - Method for preparing instant cationic high molecular weight polyacrylamide by two-step method - Google Patents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/52—Amides or imides
- C08F120/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F120/56—Acrylamide; Methacrylamide
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Abstract
The invention discloses a method for preparing instant cationic high molecular weight polyacrylamide by a two-step method, which comprises the following steps: (1) adding the dispersing agent into a reaction kettle containing a hydrocarbon solvent, and heating to dissolve the dispersing agent; (2) adding 20-40 mass% of acrylamide aqueous solution, water-soluble initiator and cationic comonomer into a reaction kettle, and stirring to form a water-in-oil reaction system; (3) introducing nitrogen to remove oxygen in the reaction system; (4) heating the reaction system to react for a period of time to form polyacrylamide primary particles; (5) dropwise adding an alcohol-water mixed solution into the reaction kettle, and stirring to ensure that polyacrylamide primary particles are aggregated to form solid particles with a structure similar to a grape bunch; (6) heating for azeotropic removal of the alcohol and water solution to obtain a high molecular weight, fast-dissolving polyacrylamide solid. The polyacrylamide obtained by the two-step method has a higher dissolution speed when in use and is not easy to agglomerate.
Description
Technical Field
The invention relates to a preparation method of high molecular weight polyacrylamide, in particular to a method for preparing instant cationic high molecular weight polyacrylamide by a two-step method.
Background
Polyacrylamide (PAM) is a linear high molecular polymer obtained by free radical polymerization of acrylamide monomers, and is widely used in the fields of oil exploitation, water treatment, chemical industry, metallurgy, paper making, and the like. Oil exploitation is the field with the largest PAM dosage in China at present. Water treatment is the second largest domestic PAM consumer area. In the aspect of municipal sewage treatment, PAM is mainly used for sludge dewatering, and a small part is used for wastewater clarification. PAM is mainly used in the paper industry as a retention aid, dry strength agent and as a flocculant for wastewater treatment. China is a large country for papermaking production and consumption, and the demand for papermaking auxiliaries is very vigorous. In addition, PAM is also well utilized in the fields of mining, coal, adhesives, leather retanning agents and the like.
Molecular weight is a key factor in determining the performance of polyacrylamide. The higher the molecular weight, the better the performance of polyacrylamide in the fields of oil exploitation, water treatment and the like. In addition, polyacrylamide is generally dissolved in an aqueous solution before use. While polyacrylamide with higher molecular weight dissolves more slowly in water. Therefore, increasing the dissolution rate can improve the performance properties of high molecular weight polyacrylamides. At present, the dissolving time of the existing polyacrylamide is basically between 1 and 2 hours, the dissolving time is long, the requirement on the process is high, the operation is complex, and the efficiency is low.
The dissolution rate of polyacrylamide particles is determined by the specific surface area of the particles and the dissolution properties of the particles themselves. The invention application with the application number of 201310257597.3 improves the dissolving speed by adding the cosolvent of ammonia water and urea. The urea is used as a common cosolvent of the polyacrylamide, although the dissolving performance of the polyacrylamide can be improved to a certain degree, the dissolving speed cannot be greatly improved, and the addition of the auxiliary agent can cause the product to contain unpleasant odor such as ammonia odor. In the invention application of application No. 201510561500.7, the dissolution rate was increased by introducing a monomer having a carboxyl group and a sulfonic acid group. Although the hydrophilicity of the carboxyl and the sulfonic group is stronger than that of the amide group, the solubility of polyacrylamide can be increased to a certain extent, but the introduction of the carboxyl and the sulfonic group of the comonomer can influence the polymerization performance of acrylamide, reduce the molecular weight of the polymer and cannot prepare the polymer with high molecular weight.
Acrylamide is a water-soluble monomer that cannot be suspension or emulsion polymerized by conventional oil-in-water (O/W) systems. Synthesis can only be carried out by inverse suspension polymerization or inverse emulsion polymerization in water-in-oil (W/O) in an organic solvent. In general, inverse emulsion polymerization gives particles having a particle size of less than 1 μm. The particle size of the inverse suspension polymerization particles is generally about several tens of microns. Such small particles are dusty during use and tend to agglomerate. Particularly, in the dissolving process, due to the large specific surface area, the water added with the water can be rapidly aggregated to form white blocks, so that the water is difficult to further dissolve, and the using effect of the water is influenced in practice.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing instant cationic high molecular weight polyacrylamide by a two-step method.
The technical scheme adopted by the invention for solving the technical problem is as follows: a method for preparing instant cationic high molecular weight polyacrylamide by a two-step method adopts a reversed phase suspension polymerization method to prepare polyacrylamide particles, and comprises the following steps:
(1) adding the dispersing agent into a reaction kettle containing a hydrocarbon solvent, and heating to dissolve the dispersing agent;
(2) adding 20-40 mass% of acrylamide aqueous solution, water-soluble initiator and cationic comonomer into the reaction kettle in the step 1, and stirring to disperse the aqueous solution in a hydrocarbon solvent to form a water-in-oil reaction system;
(3) introducing nitrogen, and removing oxygen in the reaction solution and the reaction kettle;
(4) heating the reaction system, reacting for a period of time, and then preserving heat at 75 ℃ for 1 hour to form polyacrylamide primary particles;
(5) dropwise adding an alcohol-water mixed solution into a reaction kettle, stirring, and aggregating polyacrylamide primary particles to form solid particles similar to a grape bunch structure by controlling the using amount and the alcohol-water ratio of the alcohol-water mixed solution;
(6) heating to boil, azeotropically removing alcohol and water solution to obtain high molecular weight instant polyacrylamide solid.
Further, the alcohol-water mixed solution is a mixed solution of alcohol and water, wherein the ratio of alcohol: the water ratio is 0-0.2: 1.
Furthermore, the dosage of the alcohol-water mixed solution is 10 to 200 percent of the mass of the acrylamide aqueous solution.
Further, the alcohol in the alcohol-water mixed solution is one or a mixture of methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol, ethylene glycol and propylene glycol. Methanol or ethanol is preferred.
Further, the particle size of the polyacrylamide primary particles is 50-150 μm; the particle size of the solid particles with the structure similar to the grape bunch is 0.1-1 mm.
Further, the dispersing agent is one or a mixture of several of hydrophobic nano-silica, decaglycerol decastearate, decaglycerol decaoleate, hexaglycerol pentastearate, hexaglycerol pentaoleate, sorbitan monooleate, sorbitan monostearate, glyceryl monostearate, sorbitan sesquioleate, glyceryl monostearate, diethylene glycol fatty acid ester, propylene glycol monostearate and sucrose fatty acid ester.
Further, the hydrocarbon solvent is alkane or arene of C6-C8, and can be one or more of cyclohexane, n-heptane, n-octane, isooctane, benzene and toluene.
Further, the water-soluble initiator is azobisisobutylamidine hydrochloride, azobisisobutylimidazoline hydrochloride, azobiscyanovaleric acid, azobisisopropylimidazoline, potassium persulfate, sodium persulfate, ammonium persulfate and hydrogen peroxide; and the persulfate, the peroxide, the L-ascorbic acid, the sulfite (hydrogen) salt and the ferrous salt form an oxidation-reduction system; the using amount of the water-soluble initiator is 0.0001-1 mol% of monomer acrylamide; preferably 0.005 to 0.5 mol%.
Further, the cationic comonomer is one or a mixture of more than two of acryloyloxyethyltrimethyl ammonium chloride (DAC), methacryloyloxyethyltrimethyl ammonium chloride (DMC) and dimethylamino methacryloyloxyethyltrimethyl ammonium chloride; the addition amount of the cationic comonomer is 20-150% of the mass of the acrylamide monomer.
Further, the dissolution speed of the prepared instant polyacrylamide solid is less than 20 minutes.
According to the invention, cationic polyacrylamide primary particles with the particle size of 50-150 μm are synthesized by using reverse phase suspension polymerization, and alcohol-water solution is added into a system, so that the primary particles are mutually aggregated to a certain extent, and solid particles with the particle size of 0.1-1 mm and a structure similar to a grape bunch are formed.
According to this method, an alcohol-water solution is added to the dispersed phase of primary particles after the polymerization of the monomer is completed, and water in the alcohol-water solution is adsorbed by the polyacrylamide primary particles and then swollen. As the volume of the dispersed phase (primary particles) increases, the proportion of the dispersant on the surface decreases, and the primary particles are unstable and aggregate to form particles of larger diameter (solid particles of grape-bunch structure). The addition of the alcohol solvent can control the solubility of polyacrylamide in water, prevent the polyacrylamide from being completely dissolved by water, aggregate into spherical particles, reduce the specific surface area and finally reduce the dissolution speed of the particles.
The alcohol-water ratio is controlled to be 0-0.2: 1. When the ratio exceeds 0.2: at 1, the system may be unstable and caking may occur. The dosage of the alcohol-water solution is controlled between 10 percent and 200 percent of the mass of the acrylamide water solution. When the amount of the alcohol-water solution is less than 10%, partially unagglomerated particles may appear, and finally dried to be fine powder. When the amount is more than 200%, the system may be unstable and the agglomeration phenomenon may occur due to the low ratio of the dispersant and the hydrocarbon solvent in the dispersed phase, which is a condition that must be avoided in the preparation process.
The invention has the beneficial effects that: compared with the prior art, the invention provides a method for preparing instant cationic high molecular weight polyacrylamide by a two-step method, which comprises the steps of firstly preparing primary particles with the particle size of 50-150 mu m by adopting reversed phase suspension polymerization, and then adding alcohol-water mixed liquor into a system to ensure that the primary particles are aggregated to a certain degree to obtain solid particles with the particle size of 0.1-1 mm and a structure similar to a grape bunch. The particle size and the shape of the finally obtained solid particles with the grape bunch structure can be regulated and controlled by controlling the using amount of the alcohol-water solution and the alcohol-water ratio. The solid particles with the structure of the grape bunch are aggregated together by a plurality of spherical primary particles swelled by water, the whole solid particles have larger particle size, and the special shape of the grape bunch enables the solid particles to have larger specific surface area.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
300g of cyclohexane was charged into a 1L four-necked flask, and 1.15g of sorbitan monostearate and 1g of sucrose fatty acid ester having an HLB value of 3 were added and heated to dissolve. Dissolving 95g of acrylamide and 0.8g of potassium persulfate in 200g of water by using a beaker, and adding the mixture into a four-neck flask under a nitrogen atmosphere; adding cationic comonomer DAC into a four-neck flask, wherein the dosage of the DAC is 20% of the mass of acrylamide monomer. The speed of rotation is 400rpm, nitrogen is introduced, stirring is carried out for 30 minutes, and the temperature is kept at 40 ℃. Heating to 70 ℃, reacting for 2 hours, heating to 75 ℃, and preserving heat for 1 hour. In another flask, 20g of ethanol and 100g of water were added to prepare a mixed solution. And dropwise adding the alcohol-water mixed solution into a four-neck flask, and continuously stirring for half an hour after dropwise adding is finished within half an hour. Azeotropic removal of water gave white solid particles with an average particle size of 350. mu.m.
Example 2
300g of n-hexane was added to a 1L four-necked flask, 2g of hydrophobic nano-silica and 1g of diethylene glycol fatty acid ester were added, and heated to be dissolved. Dissolving 95g of acrylamide and 0.8g of sodium persulfate in 200g of water by using a beaker, and adding the mixture into a four-neck flask under a nitrogen atmosphere; a four-neck flask was charged with cationic comonomer DMC in an amount of 30% by mass of acrylamide monomer. The speed of rotation is 400rpm, nitrogen is introduced, stirring is carried out for 30 minutes, and the temperature is kept at 40 ℃. Heating to 70 ℃, reacting for 2 hours, heating to 75 ℃, and preserving heat for 1 hour. In another flask, 6g of ethanol and 50g of water were added to prepare a mixed solution. And dropwise adding the alcohol-water mixed solution into a four-neck flask, and continuously stirring for half an hour after dropwise adding is finished within half an hour. Azeotropic removal of water gave white solid particles with an average particle size of 450. mu.m.
Example 3
300g of toluene was charged into a 1L four-necked flask, and 3g of glyceryl monostearate was added and heated to dissolve. Dissolving 95g of acrylamide and 0.8g of azobisisobutyrimidazoline hydrochloride in 200g of water by using a beaker, and adding the solution into a four-neck flask under a nitrogen atmosphere; adding a cationic comonomer of dimethylamino methacryloxyethyl trimethyl ammonium chloride into a four-neck flask, wherein the dosage of the dimethylamino methacryloxyethyl trimethyl ammonium chloride is 45% of the mass of an acrylamide monomer. The speed of rotation is 400rpm, nitrogen is introduced, stirring is carried out for 30 minutes, and the temperature is kept at 40 ℃. Heating to 60 ℃, reacting for 2 hours, heating to 75 ℃, and preserving heat for 1 hour. In another flask, 10g of isopropyl alcohol and 100g of water were added to prepare a mixed solution. And dropwise adding the alcohol-water mixed solution into a four-neck flask, and continuously stirring for half an hour after dropwise adding is finished within half an hour. Azeotropic removal of water gave white solid particles having an average particle size of 400. mu.m.
Example 4
300g of n-heptane was charged into a 1L four-necked flask, and 3g of hexaglycerol pentaoleate was added and heated to dissolve. 95g of acrylamide and 0.8g of azobiscyanovaleric acid were dissolved in 200g of water in a beaker, and the mixture was put into a four-necked flask under a nitrogen atmosphere; adding cationic comonomer DAC into a four-neck flask, wherein the dosage of the DAC is 60% of the mass of acrylamide monomer. The speed of rotation is 400rpm, nitrogen is introduced, stirring is carried out for 30 minutes, and the temperature is kept at 40 ℃. Heating to 70 ℃, reacting for 2 hours, heating to 75 ℃, and preserving heat for 1 hour. In another flask, 10g of n-butanol and 100g of water were added to prepare a mixed solution. And dropwise adding the alcohol-water mixed solution into a four-neck flask, and continuously stirring for half an hour after dropwise adding is finished within half an hour. Azeotropic removal of water gave white solid particles having an average particle size of 300. mu.m.
Example 5
300g of n-octane was put into a 1L four-necked flask, 3g of sorbitan sesquioleate was added thereto, and the mixture was heated to be dissolved. Dissolving 95g of acrylamide, 0.3g of hydrogen peroxide and 0.6g L-ascorbic acid in 200g of water by using a beaker, and adding the mixture into a four-neck flask under a nitrogen atmosphere; a four-neck flask was charged with cationic comonomer DMC in an amount of 70% by mass of acrylamide monomer. The speed of rotation is 400rpm, nitrogen is introduced, stirring is carried out for 30 minutes, and the temperature is kept at 40 ℃. Heating to 50 deg.C, reacting for 2 hr, heating to 75 deg.C, and holding for 1 hr. In another flask, 10g of ethylene glycol and 100g of water were added to prepare a mixed solution. And dropwise adding the alcohol-water mixed solution into a four-neck flask, and continuously stirring for half an hour after dropwise adding is finished within half an hour. Azeotropic removal of water gave white solid particles with an average particle size of 600. mu.m.
Comparative example 1
300g of cyclohexane was charged into a 1L four-necked flask, 1.15g of sorbitan monostearate and 1g of sucrose fatty acid ester having an HLB value of 3 were added thereto, and the mixture was heated to 60 ℃ to dissolve the sorbitan monostearate. Dissolving 95g of acrylamide and 0.8g of potassium persulfate in 200g of water by using a beaker, and adding the mixture into a four-neck flask under a nitrogen atmosphere; a four-neck flask was charged with cationic comonomer DMC in an amount of 70% by mass of acrylamide monomer. The speed of rotation is 400rpm, nitrogen is introduced, stirring is carried out for 30 minutes, and the temperature is kept at 40 ℃. Heating to 70 ℃, reacting for 2 hours, heating to 75 ℃, and preserving heat for 1 hour. Azeotropic removal of water gave white solid particles having an average particle size of 96 μm.
Dissolution Performance test
1g of polyacrylamide solid was added to 1000mL of water at 25 ℃ and stirred at 300 rpm. The time from the addition of the particles to complete dissolution of the particles is recorded as dissolution time. The properties are shown in Table 1.
| Examples | Average particle diameter of particles | Dissolution time |
| Example 1 | 350μm | 12 minutes |
| Example 2 | 450μm | 16 minutes |
| Example 3 | 400μm | 16 minutes |
| Example 4 | 300μm | 10 minutes |
| Example 5 | 600μm | 19 minutes |
| Comparative example 1 | 96μm | 73 minutes |
Wherein, the solid particles obtained in the comparative example 1 are rapidly agglomerated into block-shaped particles after being added into water, the surfaces of the agglomerated block-shaped particles can be soaked by water, and the inside of the agglomerated block-shaped particles is powdery particles and is difficult to dissolve.
The above embodiments are only for illustrating the invention and are not to be construed as limiting the invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention, therefore, all equivalent technical solutions also belong to the scope of the invention, and the scope of the invention is defined by the claims.
Claims (2)
1. A method for preparing instant cationic high molecular weight polyacrylamide by a two-step method is characterized by comprising the following steps: the preparation method of the polyacrylamide particles by adopting a reversed-phase suspension polymerization method comprises the following steps:
(1) adding the dispersing agent into a reaction kettle containing a hydrocarbon solvent, and heating to dissolve the dispersing agent;
(2) adding 20-40 mass% of acrylamide aqueous solution, water-soluble initiator and cationic comonomer into the reaction kettle in the step 1, and stirring to disperse the aqueous solution in a hydrocarbon solvent to form a water-in-oil reaction system;
(3) introducing nitrogen, and removing oxygen in the reaction solution and the reaction kettle;
(4) heating the reaction system to react for a period of time to form polyacrylamide primary particles;
(5) dropwise adding an alcohol-water mixed solution with the mass ratio of 1:10 into a reaction kettle, and stirring to ensure that polyacrylamide primary particles are aggregated to form solid particles with a structure similar to a grape bunch; the mass ratio of the using amount of the alcohol-water mixed solution to the acrylamide aqueous solution is 22: 59;
(6) heating to boil, azeotropically removing alcohol and water solution to obtain high molecular weight instant polyacrylamide solid;
the hydrocarbon solvent is one or more of cyclohexane, normal heptane, normal octane, isooctane, benzene and toluene;
the alcohol in the alcohol-water mixed solution is n-butyl alcohol or isopropanol;
the particle size of the polyacrylamide primary particles is 50-150 mu m; the particle size of the solid particles with the structure similar to the grape bunch is 0.1-1 mm; the dissolution speed of the prepared instant polyacrylamide solid is less than 20 minutes;
the dispersing agent is one or a mixture of more of hydrophobic nano-silica, decaglycerol decastearate, decaglycerol decaoleate, hexaglycerol pentastearate, hexaglycerol pentaoleate, sorbitan monooleate, sorbitan monostearate, sorbitan sesquioleate, glyceryl monostearate, diethylene glycol fatty acid ester, propylene glycol monostearate and sucrose fatty acid ester.
2. The method of claim 1 for preparing fast-dissolving cationic high molecular weight polyacrylamide in a two-step process, wherein: the water-soluble initiator is azodiisobutyl amidine hydrochloride, azodiisobutyl imidazoline hydrochloride, azodicyan valeric acid, azodiisopropyl imidazoline, potassium persulfate, sodium persulfate, ammonium persulfate and hydrogen peroxide; and the persulfate, the peroxide, the L-ascorbic acid, the sulfite (hydrogen) salt and the ferrous salt form an oxidation-reduction system; the using amount of the water-soluble initiator is 0.0001-1 mol% of monomer acrylamide;
the cationic comonomer is one or the mixture of more than two of acryloyloxyethyl trimethyl ammonium chloride (DAC), methacryloyloxyethyl trimethyl ammonium chloride (DMC) and dimethylamino methacryloyloxyethyl trimethyl ammonium chloride; the addition amount of the cationic comonomer is 20-150% of the mass of the acrylamide monomer.
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| CN101628953B (en) * | 2009-08-11 | 2012-03-21 | 华南师范大学 | High molecular weight cationic polyacrylamide preparation method |
| CN107522991B (en) * | 2017-09-27 | 2020-05-08 | 万华化学集团股份有限公司 | Super absorbent resin prepared by one-step reversed phase suspension polymerization and preparation method thereof |
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