CN109912739B - Preparation method of serial characteristic viscosity PMAPTAC - Google Patents

Preparation method of serial characteristic viscosity PMAPTAC Download PDF

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CN109912739B
CN109912739B CN201910075032.0A CN201910075032A CN109912739B CN 109912739 B CN109912739 B CN 109912739B CN 201910075032 A CN201910075032 A CN 201910075032A CN 109912739 B CN109912739 B CN 109912739B
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张跃军
王永吉
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Nanjing University of Science and Technology
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Abstract

The invention discloses a preparation method of serial characteristic viscosity PMAPTAC. The method comprises the steps of taking industrial MAPTAC as a raw material, adding triallylamine hydrochloride containing terminal double bonds or oligomer thereof with the average degree of polymerization of 0-180 and metal ion complexing agent under the condition of nitrogen atmosphere and stirring, adjusting the initial mass fraction of the monomer to be 40-72%, and corresponding peroxide initiator accounting for 0.15-0.52% of the mass fraction of the monomer, obtaining a colloid product of the PMAPTAC with high monomer conversion rate and serial characteristic viscosity through program heating, heat preservation and curing, crushing and granulating the colloid, and drying by a fluidized bed to obtain PMAPTAC dry powder with the serial characteristic viscosity of 2.0-8.2 dL/g and the monomer conversion rate of more than 99.50%.

Description

Preparation method of serial characteristic viscosity PMAPTAC
Technical Field
The invention belongs to the technical field of preparation of water-soluble cationic high-molecular compounds, and relates to a preparation method of polymethacrylamidopropyltrimethylammonium chloride (PMAPTAC) with high monomer conversion rate and serial characteristic viscosity.
Background
The cationic polymer is a water-soluble polymer with large dosage and wide application range, and can be prepared by homopolymerization of a cationic monomer, copolymerization of the cationic monomer and other olefin monomers or cationic grafting modification of a natural polymer. Among them, the polymer prepared by homopolymerization of cationic monomer has the advantages of high positive charge density and good water solubility, and is widely applied to various fields of water treatment, oil extraction, papermaking, textile and the like.
In the course of their use in these fields, it is generally accepted that, when the unit structure is determined, products of different relative molecular masses (expressed as the intrinsic viscosity) correspond to different molecular chain lengths and thus have different properties and application functions. Therefore, synthesizing a series of characteristic viscosity PMAPTAC polymers to meet different requirements of different fields on industrial application of the MAPTAC polymers with different characteristic viscosities is always a research hotspot and focus in the field. However, with the importance of resource utilization and environmental protection in modern economic society, the residual monomers in the polymer not only reduce the utilization rate of raw materials, but also generally do not play a role in application, and are often left in the environment after use, possibly causing pollution of different degrees. Therefore, from the synthesis angle, how to prepare homopolymers with adjustable intrinsic viscosity series to meet the requirements of different applications and simultaneously remarkably improve the monomer conversion rate in the polymers is a new focus and focus of research in the field.
In a cationic quaternary ammonium salt methacrylamide propyl trimethyl ammonium chloride monomer (3-methacryloylamidopropyltrimethyl ammonium chloride, MAPTAC for short), the distance between the positive ion center and a double bond is far, so that the cationic quaternary ammonium salt methacrylamide propyl trimethyl ammonium chloride monomer has higher polymerization activity, and simultaneously, the defect that an acryloyl oxygen type cationic homopolymer contains ester groups, is easy to hydrolyze and cannot play a role in an environment with a wider pH value range is overcome. The MAPTAC contains a vinyl group in a molecular structure, and can be used for producing a homopolymer Poly (3-methacrylamidopropyltrimethylammonium chloride), abbreviated as PMAPTAC, by free radical polymerization, and the reaction equation is as follows:
Figure BDA0001958477040000011
at present, only one report on the synthesis of poly (methacrylamidopropyltrimethylammonium chloride) homopolymer (PMAPTAC) is available at home and abroad. Literature (Liziqi, Ningjun, Chenglin, et al. A method for preparing high relative molecular mass homopolymers of cationic monomers of the class of acrylamidopropyltrimethylammonium chloride [ P]CN104497184A.2015-04-08.). The method adopts ammonium persulfate as an initiator and tetrasodium (Na) ethylene glycol tetraacetate4EDTA) is used as an auxiliary agent, and a polymerization process with three-step temperature rise is adopted, so that the intrinsic viscosity of the obtained product reaches 5.91 dL/g. The literature firstly discloses and reports research results of PMAPTAC homopolymer, but the product has low characteristic viscosity, is colloid, and lacks of measurement of monomer conversion rate and research report of series characteristic viscosity PMAPTAC.
From the above-mentioned research work, there are some drawbacks in the research reports on the homopolymer of PMAPTAC.
(1) So far, few research reports on homopolymer PAMPTAC at home and abroad are reported, and only literature reports adopt a three-step heating method, so that segmented polymerization of a reaction system can be realized, continuous initiation of an initiator is promoted, residual monomers are further consumed, and the characteristic viscosity and the monomer conversion rate of a product are improved, but the highest characteristic viscosity reported by the literature is only 5.91dL/g, and the characteristic viscosity of a polymer is not subjected to serial regulation and control.
(2) To date, there has been no study or report on the monomer conversion of homopolymer PMAPTAC.
(3) The PMAPTAC product reported in the literature is colloid, and is not beneficial to storage, transportation, application and popularization.
Disclosure of Invention
The invention aims to provide a preparation method of PMAPTAC with high monomer conversion rate and serial characteristic viscosity.
The technical solution for realizing the purpose of the invention is as follows:
the preparation method of the series of the characteristic viscosity PMAPTAC comprises the following specific steps:
taking an industrial monomer MAPTAC as a raw material, adding triallylamine hydrochloride or oligomer thereof containing terminal double bonds and having an average polymerization degree of 0-180 in a nitrogen atmosphere, and enabling the triallylamine hydrochloride or oligomer thereof containing the terminal double bonds to account for 0.1-5.0% of the mass fraction of the monomer; adjusting the initial mass fraction of the monomer to be 40-72%, adding a peroxide initiator accounting for 0.15-0.52% of the mass fraction of the monomer, adding a metal ion complexing agent, stirring and mixing uniformly, heating the reaction solution by a program to initiate polymerization reaction at the sectional initiation temperatures of 35-45 ℃, 45-55 ℃ and 65-75 ℃, and carrying out thermal polymerization to obtain a PMAPTAC colloidal product with a series of characteristic viscosities; and granulating and drying the colloid to obtain the PMAPTAC dry powder with high conversion rate and serial characteristic viscosity.
The content of the industrial monomer MAPTAC (calculated by mass fraction, the same below) is 75-85%.
The metal ion complexing agent is tetrasodium ethylene diamine tetraacetate or disodium ethylene diamine tetraacetate, and accounts for 0.025-0.06 percent of the mass fraction of the monomer.
The peroxide initiator is ammonium persulfate or sodium persulfate or potassium persulfate.
The polymerization time under the condition of heat preservation is 3.0 plus or minus 0.5 h.
The drying is carried out at 70-110 ℃ by a fluidized bed.
The drying time is 1.0 plus or minus 0.5 h.
Compared with the prior art, the invention has the following remarkable advantages:
(1) the relationship between monomer and initiator concentration can be calculated for polymers of increasing chain length according to the kinetic chain length equation (equation 1) (polymer chemistry, fifth edition, eds.; 2013): when the relative molecular mass of the polymer is required to be increased, namely the average polymerization degree is increased by 1.6-1.4 times, and the kinetic chain length is also increased by 1.6-1.4 times, if the monomer concentration is controlled to be increased by 22%, the initiator concentration is decreased by 42% -24%, and then the polymerization product with the required serial characteristic viscosity and high monomer conversion rate can be obtained. Therefore, in combination with the preliminary optimization exploration of experimental conditions, the initial mass fraction of the selected monomer is increased from 40% to 72%, and the corresponding initiator addition amount accounts for 0.52% and is reduced to 0.15% of the mass fraction of the monomer, so that the preparation of the target PMAPTAC dry powder product with the series of intrinsic viscosities ranging from 2.0dL/g to 8.2dL/g and the monomer conversion rate of more than 99.50% is realized. The preparation of the PMAPTAC product with high monomer conversion rate and relative molecular mass in series can obviously improve the utilization rate of raw materials, greatly expand the application range, can be widely applied to multiple fields of oil exploitation, papermaking, mining, textile printing and dyeing, daily chemical industry, water treatment and the like, and provides unique environment-friendly property for the series products due to high monomer conversion rate (less residual monomers).
Figure BDA0001958477040000031
(2) The compound with weak reactivity and containing terminal group double bonds is added, so that the compound exists stably at low temperature, the process of a rapid reaction stage is not influenced, the reaction is carried out at high temperature, particularly in a drying stage, namely, a chain extender is added, residual monomers and polymers are easily connected, and the characteristic viscosity loss caused by high-temperature degradation is counteracted. The compounds containing terminal double bonds exert their aforementioned effects sufficiently under the process conditions of the present invention to further increase the intrinsic viscosity and monomer conversion of the polymer PMAPTAC.
(3) The PMAPTAC colloidal product is granulated and dried by a fluidized bed to prepare dry powder, so that the product is convenient to store and transport, and the application and popularization of PMAPTAC homopolymer are facilitated.
Detailed Description
The technique of the present invention will be described below with reference to examples.
Example 1
Firstly, feeding a 75% MAPTAC monomer aqueous solution into a polymerization reactor with a thermometer, a stirring device and a nitrogen introducing device, and adding an oligomer triallylamine hydrochloride homopolymer with the average polymerization degree of 180 under the stirring of nitrogen atmosphere to account for (5.00 +/-0.01)% of the mass fraction of the monomers;
secondly, adding a metal complexing agent ethylenediaminetetraacetic acid tetrasodium solution accounting for 0.06 +/-0.005 percent of the mass fraction of the monomer and a sodium persulfate initiator solution accounting for 0.52 +/-0.01 percent of the mass fraction of the monomer into the aqueous solution, and adding water to adjust the mixture to obtain a reaction solution with the initial mass fraction of the monomer of (40 +/-1)%;
thirdly, after stirring for 20min in nitrogen atmosphere, firstly heating the reaction solution to (35.0 +/-1.0) DEG C to initiate polymerization, and keeping the temperature for polymerization for (3.0 +/-0.5) h;
fourthly, heating the reaction system to 47.0 +/-1.0 ℃ and keeping the polymerization time at (3.0 +/-0.5) h;
fifthly, finally heating the reaction system to 68.0 +/-2.0 ℃ and stopping heating after the polymerization time is 3.0 +/-0.5 hours;
sixthly, cooling and discharging the PMAPTAC colloid product, crushing and granulating the colloid, drying the colloid product by a fluidized bed at the temperature of 70 +/-5 ℃ for 1.0 +/-0.5 h to obtain a PMAPTAC dry powder product, measuring the product in a solution of 30.0 +/-0.1 ℃ and 1.0mol/LNaCl by using an Ubbelohde viscometer to obtain the product with the characteristic viscosity value of 2.0dL/g, and measuring the monomer conversion rate by a bromination method to be 99.50%.
Example 2
Firstly, feeding an aqueous MAPTAC monomer solution with the content of 80% into a polymerization reactor with a thermometer, a stirring device and a nitrogen introducing device, and adding an oligomer triallylamine hydrochloride homopolymer with the average polymerization degree of 120 into the polymerization reactor under the stirring of nitrogen atmosphere to enable the oligomer triallylamine hydrochloride homopolymer to account for (4.50 +/-0.01)% of the mass fraction of the monomers;
secondly, adding a metal complexing agent disodium ethylene diamine tetraacetate solution accounting for 0.051 +/-0.005 percent of the mass fraction of the monomer and a potassium persulfate initiator solution accounting for 0.31 +/-0.02 percent of the mass fraction of the monomer into the aqueous solution, and adding water to adjust to obtain a reaction solution with the initial mass fraction of the monomer of 48.8 +/-1.0 percent;
thirdly, after stirring for 20min in nitrogen atmosphere, firstly heating the reaction solution to (40.5 +/-1.0) DEG C to initiate polymerization, and keeping the temperature for polymerization for (3.0 +/-0.5) h;
fourthly, heating the reaction system to 53.0 +/-1.0 ℃ and keeping the temperature for polymerization for 3.0 +/-0.5 hours;
fifthly, finally heating the reaction system to 75.0 +/-1.0 ℃ and stopping heating after the polymerization time is 3.0 +/-0.5 hours;
sixthly, cooling and discharging the PMAPTAC colloid product, crushing and granulating the colloid, drying the colloid product by a fluidized bed at the temperature of 90 +/-5 ℃ for 1.0 +/-0.5 h to obtain a PMAPTAC dry powder product, measuring the product in a solution of 30.0 +/-0.1 ℃ and 1.0mol/LNaCl by using an Ubbelohde viscometer to obtain the product with the characteristic viscosity value of 4.12dL/g, and measuring the monomer conversion rate by a bromination method to be 99.67%.
Example 3
Firstly, feeding a MAPTAC monomer aqueous solution with the content of 85% into a polymerization reactor with a thermometer, a stirring device and a nitrogen introducing device, and adding an oligomer triallylamine hydrochloride homopolymer with the average polymerization degree of 80 into the polymerization reactor under the stirring of nitrogen atmosphere to enable the oligomer triallylamine hydrochloride homopolymer to account for (1.50 +/-0.01)% of the mass fraction of the monomer;
secondly, adding a metal complexing agent ethylene diamine tetraacetic acid tetrasodium solution accounting for 0.04 +/-0.005 percent of the mass fraction of the monomer and an ammonium persulfate initiator solution accounting for 0.20 +/-0.01 percent of the mass fraction of the monomer into the aqueous solution, and adding water to adjust to obtain a reaction solution with the initial mass fraction of the monomer of (59.5 +/-1.0 percent);
thirdly, after stirring for 20min in nitrogen atmosphere, firstly heating the reaction solution to 45.0 +/-1.0 ℃ to initiate polymerization, and keeping the temperature for polymerization for 3.0 +/-0.5 h;
fourthly, heating the reaction system to 55.0 +/-1.0 ℃ and keeping the polymerization time at 3.0 +/-0.5 h;
fifthly, finally heating the reaction system to (65.0 +/-1.0) DEG C, keeping the temperature for polymerization for (3.0 +/-0.5) h, and then stopping heating;
sixthly, cooling and discharging the PMAPTAC colloid product, crushing and granulating the colloid, drying the colloid product by a fluidized bed at the temperature of 100 +/-5 ℃ for 1.0 +/-0.5 h to obtain a PMAPTAC dry powder product, measuring the product in a solution of 30.0 +/-0.1 ℃ and 1.0mol/LNaCl by using an Ubbelohde viscometer to obtain the product with the characteristic viscosity value of 5.94dL/g, and measuring the monomer conversion rate by a bromination method to be 99.73%.
Example 4
Firstly, feeding a MAPTAC monomer aqueous solution with the content of 80% into a polymerization reactor with a thermometer, a stirring device and a nitrogen introducing device, and adding a triallylamine hydrochloride monomer with the average polymerization degree of 0 under the stirring of nitrogen atmosphere to enable the triallylamine hydrochloride monomer to account for (0.10 +/-0.01)% of the mass fraction of the monomer;
secondly, adding a metal complexing agent ethylene diamine tetraacetic acid tetrasodium solution accounting for 0.025 +/-0.005 percent of the mass fraction of the monomer and an ammonium persulfate initiator solution accounting for 0.15 +/-0.01 percent of the mass fraction of the monomer into the aqueous solution, and adding water to adjust to obtain a reaction solution with the initial mass fraction of the monomer of 72.6 +/-1.0 percent;
thirdly, after stirring for 20min in nitrogen atmosphere, firstly heating the reaction solution to (40.0 +/-1.0) DEG C to initiate polymerization, and keeping the temperature for polymerization for (3.0 +/-0.5) h;
fourthly, heating the reaction system to 50.0 +/-1.0 ℃ and keeping the temperature for polymerization for 3.0 +/-0.5 hours;
fifthly, finally heating the reaction system to (71.0 +/-1.0) DEG C, keeping the temperature for polymerization for (3.0 +/-0.5) h, and then stopping heating;
sixthly, cooling and discharging the PMAPTAC colloid product, crushing and granulating the colloid, drying the colloid product by a fluidized bed at the temperature of 110 +/-5 ℃ for 1.0 +/-0.5 h to obtain a PMAPTAC dry powder product, measuring the product in a solution of 30.0 +/-0.1 ℃ and 1.0mol/LNaCl by using an Ubbelohde viscometer to obtain the product with the characteristic viscosity value of 8.2dL/g, and measuring the monomer conversion rate by a bromination method to be 99.88%.
Comparative example 1
This comparative example is essentially the same as example 3, except that the average degree of polymerization of the triallylamine hydrochloride homopolymer added is 260, as follows:
firstly, feeding a MAPTAC monomer aqueous solution with the content of 85% into a polymerization reactor with a thermometer, a stirring device and a nitrogen introducing device, and adding an oligomer triallylamine hydrochloride homopolymer with the average polymerization degree of 260 under the stirring of nitrogen atmosphere to account for (1.50 +/-0.01)% of the mass fraction of the monomer;
secondly, adding a metal complexing agent ethylene diamine tetraacetic acid tetrasodium solution accounting for 0.04 +/-0.005 percent of the mass fraction of the monomer and an ammonium persulfate initiator solution accounting for 0.20 +/-0.01 percent of the mass fraction of the monomer into the aqueous solution, and adding water to adjust to obtain a reaction solution with the initial mass fraction of the monomer of (59.5 +/-1.0 percent);
thirdly, after stirring for 20min in nitrogen atmosphere, firstly heating the reaction solution to 45.0 +/-1.0 ℃ to initiate polymerization, and keeping the temperature for polymerization for 3.0 +/-0.5 h;
fourthly, heating the reaction system to 55.0 +/-1.0 ℃ and keeping the polymerization time at 3.0 +/-0.5 h;
fifthly, finally heating the reaction system to (65.0 +/-1.0) DEG C, keeping the temperature for polymerization for (3.0 +/-0.5) h, and then stopping heating;
sixthly, cooling and discharging the PMAPTAC colloid product, crushing and granulating the colloid, drying the colloid product by a fluidized bed at the temperature of 100 +/-5 ℃ for 1.0 +/-0.5 h to obtain a PMAPTAC dry powder product, measuring the product in a solution of 30.0 +/-0.1 ℃ and 1.0mol/LNaCl by using an Ubbelohde viscometer to obtain the product with the characteristic viscosity value of 3.56dL/g, and measuring the monomer conversion rate of 97.72% by using a bromination method.
Comparative example 2
This comparative example is essentially the same as example 3, except that the mass ratio of the triallylamine hydrochloride homopolymer added to the monomers was (6.40. + -. 0.01)%, and the specific procedure was as follows:
firstly, feeding a MAPTAC monomer aqueous solution with the content of 85% into a polymerization reactor with a thermometer, a stirring device and a nitrogen introducing device, and adding an oligomer triallylamine hydrochloride homopolymer with the average polymerization degree of 80 into the polymerization reactor under the stirring of nitrogen atmosphere to enable the oligomer triallylamine hydrochloride homopolymer to account for (6.40 +/-0.01)% of the mass fraction of the monomer;
secondly, adding a metal complexing agent ethylene diamine tetraacetic acid tetrasodium solution accounting for 0.04 +/-0.005 percent of the mass fraction of the monomer and an ammonium persulfate initiator solution accounting for 0.20 +/-0.01 percent of the mass fraction of the monomer into the aqueous solution, and adding water to adjust to obtain a reaction solution with the initial mass fraction of the monomer of (59.5 +/-1.0 percent);
thirdly, after stirring for 20min in nitrogen atmosphere, firstly heating the reaction solution to (40.5 +/-1.0) DEG C to initiate polymerization, and keeping the temperature for polymerization for (3.0 +/-0.5) h;
fourthly, heating the reaction system to 51.0 +/-1.0 ℃ and keeping the polymerization time at 3.0 +/-0.5 h;
fifthly, finally heating the reaction system to 70.0 +/-2.0 ℃ and stopping heating after the polymerization time is 3.0 +/-0.5 hours;
sixthly, cooling and discharging the PMAPTAC colloid product, crushing and granulating the colloid, drying the colloid product by a fluidized bed at the temperature of 100 +/-5 ℃ for 1.0 +/-0.5 h to obtain a PMAPTAC dry powder product, measuring the product in a solution of 30.0 +/-0.1 ℃ and 1.0mol/LNaCl by using an Ubbelohde viscometer to obtain the product with the characteristic viscosity value of 4.02dL/g, and measuring the monomer conversion rate of 97.08% by using a bromination method.
Comparative example 3
This comparative example is essentially the same as example 4, except that no triallylamine hydrochloride monomer was added to the system, as follows:
firstly, feeding a MAPTAC monomer aqueous solution with the content of 80% into a polymerization reactor with a thermometer, a stirring device and a nitrogen introducing device, adding a metal complexing agent-ethylene diamine tetraacetic acid tetrasodium solution accounting for 0.025 +/-0.005)% of the mass fraction of the monomer and an ammonium persulfate initiator solution accounting for 0.15 +/-0.01)% of the mass fraction of the monomer under the stirring of nitrogen atmosphere, and adding water for regulation to obtain a reaction solution with the initial mass fraction of the monomer of (72.6 +/-1.0)%;
secondly, after stirring for 20min under the nitrogen atmosphere, firstly heating the reaction solution to (40.0 +/-1.0) DEG C to initiate polymerization, and keeping the temperature for polymerization for (3.0 +/-0.5) h;
thirdly, heating the reaction system to 50.0 +/-1.0 ℃ and keeping the polymerization time at 3.0 +/-0.5 h;
fourthly, finally heating the reaction system to 71.0 +/-1.0 ℃ and stopping heating after the polymerization time is 3.0 +/-0.5 hours;
fifthly, cooling and discharging the PMAPTAC colloid product, crushing and granulating the colloid, drying the colloid product by a fluidized bed at the temperature of 110 +/-5 ℃ for 1.0 +/-0.5 h to obtain a PMAPTAC dry powder product, measuring the product in a solution of 30.0 +/-0.1 ℃ and 1.0mol/LNaCl by using an Ubbelohde viscometer to obtain the product with the characteristic viscosity value of 3.98dL/g, and measuring the monomer conversion rate by a bromination method to 97.87%.

Claims (8)

1. The preparation method of the series of the characteristic viscosity PMAPTAC is characterized by comprising the following specific steps of:
taking an industrial monomer MAPTAC as a raw material, adding triallylamine hydrochloride or oligomer thereof containing terminal double bonds and having an average polymerization degree of 0-180 in a nitrogen atmosphere, and enabling the triallylamine hydrochloride or oligomer thereof containing the terminal double bonds to account for 0.1-5.0% of the mass fraction of the monomer; adding water to adjust the initial mass fraction of the monomer to be 40-72%, adding a peroxide initiator accounting for 0.15-0.52% of the mass fraction of the monomer, adding a metal ion complexing agent, stirring and mixing uniformly, heating the reaction solution by stages through a program to initiate polymerization reaction, wherein the stage initiation temperatures are 35-45 ℃, 45-55 ℃ and 65-75 ℃, and carrying out heat preservation polymerization to obtain a PMAPTAC colloidal product with a series of characteristic viscosities; and granulating and drying the colloid to obtain the PMAPTAC dry powder with high conversion rate and serial characteristic viscosity.
2. The method of claim 1, wherein the industrial monomer MAPTAC content in the raw material is 75-85%.
3. The method of claim 1, wherein the metal ion complexing agent is tetrasodium ethylenediaminetetraacetate or disodium ethylenediaminetetraacetate.
4. The preparation method according to claim 1, wherein the metal ion complexing agent accounts for 0.025-0.06% of the mass fraction of the monomer.
5. The process according to claim 1, wherein the peroxide initiator is ammonium persulfate or sodium persulfate or potassium persulfate.
6. The method according to claim 1, wherein the polymerization time is 3.0 ± 0.5 h.
7. The preparation method according to claim 1, wherein the drying is fluidized bed drying at 70-110 ℃.
8. The method of claim 1, wherein the drying time is 1.0 ± 0.5 h.
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