CN103073680B - Synthetic method of ultraviolet initiated hydrophobic modified cationic polyacrylamide - Google Patents
Synthetic method of ultraviolet initiated hydrophobic modified cationic polyacrylamide Download PDFInfo
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Abstract
The invention provides a synthetic method of ultraviolet initiated hydrophobic modified cationic polyacrylamide, which comprises the steps of sequentially adding deionized water, a cationic monomer, a hydrophobic monomer and an acrylamide monomer in a reaction device, uniformly stirring till the deionized water, the cationic monomer, the hydrophobic monomer and the acrylamide monomer are completely dissolved to form a monomer aqueous solution, adding an appropriate cosolvent and an initiating agent in the monomer aqueous solution, uniformly stirring, adjusting a pH (potential of hydrogen) value, filling high-purity nitrogen in the reaction device to exhaust air from the reaction device, placing the reaction device in an ultraviolet reaction device to initiate a polymerization reaction after the reaction device is sealed, generating hydrophobic modified cationic polyacrylamide colloid, purifying, washing and refining the colloid, drying in a vacuum drying oven, grinding, and obtaining ultraviolet initiated hydrophobic modified cationic polyacrylamide. According to the method, the initiated polymerization time is short; heating or cooling control is not required; in this case, the production technology is simplified; the energy consumption is reduced; and the production cost is lowered.
Description
Technical field
The present invention relates to a kind of synthetic method of high molecular weight water soluble polymer, be specifically related to the synthetic method that a kind of UV-light causes dewatered modified cation polyacrylamide.
Background technology
At present, the flocculation agent for waste water and sludge dewatering treatment is mainly organic polymer coargulator, compares inorganic flocculating agent, and organic polymer coargulator has that consumption is few, pH value of sewage water impact is little, flocculation rate fast, coexisted the advantages such as salt.Polyacrylamide be apply more extensive, the synthesis class water-soluble high-molecular compound that whole world consumption is maximum, PAM can be divided into anion-polyacrylamide according to PAM side chain Suo Dai functional group, cationic-type polyacrylamide and non-ionic polyacrylamide three kinds, wherein cationic-type polyacrylamide is a kind of efficient flocculant, dewatered modified cation polyacrylamide makes in cation polypropylene acyl containing hydrophobic grouping because its large hydrophilic molecular chain introducing a small amount of hydrophobic grouping, there is stronger heat resistance and salt tolerance, with hydrophobic association, adsorption bridging and electrical counteract effect, be widely used in municipal effluent, industrial sewage and sludge dewatering treatment process.
At present, dewatered modified cation polyacrylamide synthetic method is mainly divided into: the methods etc. such as micellar copolymerization, polymerization in homogeneous phase and dispersion polymerization.In these synthetic methods, mainly have the following disadvantages: 1, reaction times overlong time, great majority are by water-bath constant temp. heating initiation method, as " a kind of hydrophobic associated polymer and preparation method thereof and application " that patent publication No. is CN101260174A, hydrophobic associated polymer is obtained by polyreaction, its 4 ~ 12 hours consuming time, initiated polymerization overlong time.And for example patent publication No. is " a kind of synthetic method of hydrophobic association polyacrylamide " of CN102796222A, and be by obtained hydrophobic association acrylamide 6 ~ 8 hours consuming time, polymerization time is also long.2, need in elicitation procedure to add stablizer, moieties also has certain toxicity, as threat certain to the healthy formation of people during water treatment.As " a kind of synthetic method of hydrophobic association polyacrylamide " that patent publication No. is CN102796222A, need to add trimeric cyanamide, dicyandiamide etc.
Summary of the invention
For prior art above shortcomings, the present invention solves long reaction time in the building-up process of cationic polyacrylamide, needs to use the problem of toxicant, provides the synthetic method of the dewatered modified cation polyacrylamide that a kind of velocity of initiation is fast, use safety, production cost are lower.
Solve the problems of the technologies described above, the present invention adopts following technical scheme to realize: a kind of UV-light causes the synthetic method of dewatered modified cation polyacrylamide, comprises the following steps:
The first step, deionized water, cationic monomer is added successively in reaction unit, hydrophobic monomer and acrylamide monomer stir to dissolving formation monomer solution completely, wherein deionized water is as solvent, meter cationic monomer, hydrophobic monomer and acrylamide monomer are total monomer, and meter cationic monomer and acrylamide monomer are total water-soluble monomer; In described monomer solution, total monomer quality mark is 10% ~ 50%, and the mass percent of described cationic monomer and acrylamide monomer is 5% ~ 90%:10% ~ 95%, and described hydrophobic monomer accounts for 2% ~ 10% of total water-soluble mono weight;
Second step, in above-mentioned monomer solution, add account for total water-soluble mono weight 0.2% ~ 2% urea as solubility promoter, add account for total water-soluble mono weight 1% ~ 6% cetyl trimethylammonium bromide as tensio-active agent, add the initiator accounting for total water-soluble mono weight 0.1 ‰ ~ 0.8 ‰, be uniformly mixed, then add mineral acid and the pH value of monomer solution is adjusted to 2. ~ 6 by mineral alkali; Then be filled with High Purity Nitrogen to reaction unit, after the air in reaction unit is got rid of completely, reaction unit sealed; Impurity in air and oxygen, especially oxygen can hinder polyreaction, therefore in order to be realize polyreaction better, accelerate polymerization rate, being filled with High Purity Nitrogen the air in reaction unit is completed eliminating in reaction unit;
3rd step, under Interior Temperature Environment, puts into UV-light reaction unit by the reaction unit after sealing in second step, initiated polymerization is carried out under UV-irradiation, take out after 20min ~ 80min, leave standstill slaking more than 1 hour, obtained gluey dewatered modified cation polyacrylamide;
4th step, particulate state made by the gluey dewatered modified cation polyacrylamide 3rd step obtained, stir and be dissolved in deionized water completely, re-use to amass and purify than for the dehydrated alcohol of 2:1 and the mixed solutions for many times of acetone, wash, refine, then grinding after drying in vacuum drying oven, obtains dewatered modified cation Polyacrylamide Powder.
Further, the cationic monomer in the described the first step is acrylyl oxy-ethyl-trimethyl salmiac or MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride.MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, English Methacryloxyethyltrimethyl Ammonium Chloride by name, is called for short DMC; Acrylyl oxy-ethyl-trimethyl salmiac DAC, English Acryloxyethyl Trimethyl Ammonium Chloride by name is called for short DAC, and these two kinds of monomers are conventional commercially available cationic monomer, easily obtain, and can homopolymerization or copolymerization.
Hydrophobic monomer in the described the first step is butyl acrylate, octadecyl acrylate or dimethylaminoethyl methacrylate.Introduce hydrophobic monomer, due on its main chain containing hydrophobic grouping, when polymkeric substance is water-soluble, the hydrophobic grouping in polymkeric substance and assembling between the hydrophobic grouping of Organic substance in water, forms small water repellent region, generation heat resistance and salt tolerance.Heat resistance and salt tolerance causes Organic substance in water generation adsorpting aggregation, and this effect causes that dewatered modified cation polyacrylamide is more fast to Organic substance in water adsorpting aggregation, adsorptive capacity is larger, strengthens the ability removing Organic substance in water.Have good application prospect at sewage treatment area, apply to some extent at paper waste, petrochemical wastewater, dyeing waste water, leather-making waste water etc., treatment effect is better than conventional flocculant.
Initiator in described second step is azo-bis-isobutyrate hydrochloride V-50 or azo two isobutyl imidazoline hydrochloride VA-044.Azo-bis-isobutyrate hydrochloride V-50 or azo two isobutyl imidazoline hydrochloride VA-044 is the water-soluble azo initiator of typical mature, the decomposition reaction of these two kinds of initiators is first order reaction, without induced decomposition, just can initiated polymerization under lower concentration and temperature, consumption is few, and efficiency of initiation is high, reacting balance, less residue, is conducive to the purity and the molecular weight that improve product; And these two kinds of initiators are more stable, be convenient to store.
Initiator in described second step is composite initiator, this composite initiator is made up of organic initiators and inorganic initiator, wherein organic initiators is azo-bis-isobutyrate hydrochloride V-50 or azo two isobutyl imidazoline hydrochloride VA-044, and inorganic initiator is ammonium persulphate and sodium bisulfite; The mass ratio of described ammonium persulphate, organic initiators and sodium bisulfite is (2 ~ 4): (1 ~ 2): (1 ~ 2).Azo-bis-isobutyrate hydrochloride V-50 or azo two isobutyl imidazoline hydrochloride VA-044 is that photoinitiator can be got together by trigger monomer fast under UV-irradiation, because redox system activation energy is lower, redox initiation system and organic initiators is adopted to form composite initiator, can at low temperature initiated polymerization, when can make the intensity of polymerization initial stage UV-light for reaching nominal strength like this, initiated polymerization, improves efficiency of initiation, accelerate velocity of initiation, reduce the initiated polymerization time.
Further, in described second step UV-light produced by high voltage mercury lamp, and produce ultraviolet wavelength be 200nm ~ 400nm, predominant wavelength is 365nm, and light intensity is 600 ~ 1800 uw/cm
2.The UV-light of this wave band has stronger penetrativity, reaction unit can be penetrated initiated polymerization is carried out to mixed solution wherein, and can polymerization rate be improved, shorten polymerization reaction time, this UV-light reaction unit has the advantage such as easy and simple to handle, energy-conserving and environment-protective, practical safety.
Compared to existing technology, the present invention has following beneficial effect:
1, generated time is shorter.The present invention adopts uv-light polymerization, UV-light can be accelerated initiator and equal schizogenesis occurs, once generate primary group of free radicals, itself and monomer just can carry out addition fast, monomer radical just obtains, polymerization rate is just accelerated greatly, so can greatly shorten the initiated polymerization time, its initiated polymerization time is minimum reaches 25min.
2, adopt the method that the invention provides to prepare dewatered modified cation polyacrylamide not need to add stablizer, obtained Product Safety is high.
3, synthetic method provided by the invention is not owing to needing to control temperature, at room temperature just can polyreaction,
Therefore avoid due to too high or too low for temperature on the impact of polyreaction, not only simply energy-conservation, and also preparation process easily controls.
4, the starting material selected by synthetic method provided by the invention are commercially available material, cheap, choose conveniently, can
Direct purchase, therefore, production cost is low.
5, the finished product that the present invention produces can be widely used in the industries such as water treatment, papermaking, ore dressing, oil production, weaving, medicine.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Adopt HCl as mineral acid in following examples, NaOH is as mineral alkali adjust ph, also can adopt during concrete enforcement in prior art that other do not affect mineral acid and the mineral alkali adjust ph of polyreaction, the indoor environment temperature that polyreaction uses is 5 DEG C ~ 30 DEG C room temps.
embodiment 1:uV-light causes a synthetic method for dewatered modified cation polyacrylamide, it is characterized in that, comprises the following steps:
The first step, deionized water 91.8ml is added successively in reaction unit, acrylyl oxy-ethyl-trimethyl salmiac monomer (DAC) 0.5g, Butyl Acrylate Monomer (BA) 0.2g and acrylamide monomer (AM) 9.5 g stirs to dissolving formation monomer solution completely, wherein deionized water is as solvent, meter acrylyl oxy-ethyl-trimethyl salmiac monomer (DAC), Butyl Acrylate Monomer (BA) and acrylamide monomer (AM) are total monomer, meter acrylyl oxy-ethyl-trimethyl salmiac monomer (DAC) and acrylamide monomer (AM) are total water-soluble monomer, in monomer solution, total monomer quality mark is 10%, and the mass percent of acrylyl oxy-ethyl-trimethyl salmiac monomer and acrylamide monomer is 5%:95%, and Butyl Acrylate Monomer accounts for 2% of total water-soluble mono weight,
Second step, in above-mentioned monomer solution, add account for total water-soluble mono weight 0.2% urea as solubility promoter, add account for total water-soluble mono weight 1.0% cetyl trimethylammonium bromide (CTAB) as tensio-active agent, add account for total water-soluble mono weight 0.1 ‰ azo-bis-isobutyrate hydrochloride V-50 as initiator, be uniformly mixed, then add mineral acid and the pH value of monomer solution is adjusted to 2. by mineral alkali; Then be filled with High Purity Nitrogen to reaction unit, after the air in reaction unit is got rid of completely, reaction unit sealed;
3rd step, under Interior Temperature Environment, reaction unit after sealing in second step is put into UV-light reaction unit, initiated polymerization is carried out under UV-irradiation, wavelength 200nm ~ the 400nm sent by high voltage mercury lamp during this UV-light, the UV-light of predominant wavelength 365nm, takes out after 20min, leave standstill slaking more than 1 hour, obtained gluey dewatered modified cation polyacrylamide;
4th step, particulate state made by the gluey dewatered modified cation polyacrylamide 3rd step obtained, long-pending ratio is used to be that the dehydrated alcohol of 2:1 and the mixing solutions of acetone are purified for three times, wash, refined, then grinding after drying in vacuum drying oven, obtains dewatered modified cation Polyacrylamide Powder.
Employing colloid titration method detects, and the limiting viscosity recording the dewatered modified cation polyacrylamide finally obtained is 2064.5 mL/g, and solid content is 29.9%, and cationic degree is 5 %.
embodiment 2:uV-light causes a synthetic method for dewatered modified cation polyacrylamide, it is characterized in that, comprises the following steps:
The first step, deionized water 24.5ml, acrylyl oxy-ethyl-trimethyl salmiac monomer (DAC) 3g is added successively in reaction unit, Butyl Acrylate Monomer (BA) 0.5g and acrylamide monomer (AM) 7 g stirs to dissolving formation monomer solution completely, wherein deionized water is as solvent, meter acrylyl oxy-ethyl-trimethyl salmiac monomer (DAC), Butyl Acrylate Monomer (BA) and acrylamide monomer (AM) are total monomer, and meter acrylyl oxy-ethyl-trimethyl salmiac monomer (DAC) and acrylamide monomer (AM) are total water-soluble monomer; In monomer solution, total monomer quality mark is 30%, and the mass percent of acrylyl oxy-ethyl-trimethyl salmiac monomer and acrylamide monomer is 30%:70%, and Butyl Acrylate Monomer accounts for 5% of total water-soluble mono weight;
Second step, in above-mentioned monomer solution, add account for total water-soluble mono weight 1.0% urea as solubility promoter, add account for total water-soluble mono weight 2.0% cetyl trimethylammonium bromide (CTAB) as tensio-active agent, add the composite initiator accounting for total water-soluble mono weight 0.7 ‰, in this composite initiator, the mass ratio of ammonium persulphate, sodium bisulfite and azo-bis-isobutyrate hydrochloride V-50 is 2:1:1, be uniformly mixed, then add mineral acid and the pH value of monomer solution is adjusted to 3.5. by mineral alkali; Then be filled with High Purity Nitrogen to reaction unit, after the air in reaction unit is got rid of completely, reaction unit sealed;
3rd step, under Interior Temperature Environment, reaction unit after sealing in second step is put into UV-light reaction unit, initiated polymerization is carried out under UV-irradiation, wavelength 200nm ~ the 400nm sent by high voltage mercury lamp during this UV-light, the UV-light of predominant wavelength 365nm, takes out after 60min, leave standstill slaking more than 1 hour, obtained gluey dewatered modified cation polyacrylamide;
4th step, particulate state made by the gluey dewatered modified cation polyacrylamide 3rd step obtained, long-pending ratio is used to be that the dehydrated alcohol of 2:1 and the mixing solutions of acetone are purified for three times, wash, refined, then grinding after drying in vacuum drying oven, obtains dewatered modified cation Polyacrylamide Powder.
Employing colloid titration method detects, and the limiting viscosity recording the dewatered modified cation polyacrylamide finally obtained is 1860.0 mL/g, and solid content is 29.8%, and cationic degree is 30.0%.
embodiment 3:uV-light causes a synthetic method for dewatered modified cation polyacrylamide, it is characterized in that, comprises the following steps:
The first step, deionized water 11.0ml is added successively in reaction unit, acrylyl oxy-ethyl-trimethyl salmiac monomer (DAC) 9.0 g, Butyl Acrylate Monomer (BA) 1.0g and acrylamide monomer (AM) 1.0 g stirs to dissolving formation monomer solution completely, wherein deionized water is as solvent, meter acrylyl oxy-ethyl-trimethyl salmiac monomer (DAC), Butyl Acrylate Monomer (BA) and acrylamide monomer (AM) are total monomer, meter acrylyl oxy-ethyl-trimethyl salmiac monomer (DAC) and acrylamide monomer (AM) are total water-soluble monomer, in monomer solution, total monomer quality mark is 50%, and the mass percent of acrylyl oxy-ethyl-trimethyl salmiac monomer and acrylamide monomer is 90%:10%, and Butyl Acrylate Monomer accounts for 10% of total water-soluble mono weight,
Second step, in above-mentioned monomer solution, add account for total water-soluble mono weight 2.0% urea as solubility promoter, add account for total water-soluble mono weight 6.0% cetyl trimethylammonium bromide (CTAB) as tensio-active agent, add account for total water-soluble mono weight 0.8 ‰ azo-bis-isobutyrate hydrochloride V-50 as initiator, be uniformly mixed, then add mineral acid and the pH value of monomer solution is adjusted to 6. by mineral alkali; Then be filled with High Purity Nitrogen to reaction unit, after the air in reaction unit is got rid of completely, reaction unit sealed;
3rd step, under Interior Temperature Environment, reaction unit after sealing in second step is put into UV-light reaction unit, initiated polymerization is carried out under UV-irradiation, wavelength 200nm ~ the 400nm sent by high voltage mercury lamp during this UV-light, the UV-light of predominant wavelength 365nm, takes out after 80min, leave standstill slaking more than 1 hour, obtained gluey dewatered modified cation polyacrylamide;
4th step, particulate state made by the gluey dewatered modified cation polyacrylamide 3rd step obtained, long-pending ratio is used to be that the dehydrated alcohol of 2:1 and the mixing solutions of acetone are purified for three times, wash, refined, then grinding after drying in vacuum drying oven, obtains dewatered modified cation Polyacrylamide Powder.
Employing colloid titration method detects, and the limiting viscosity recording the dewatered modified cation polyacrylamide finally obtained is 761.2mL/g, and solid content is 26.3%, and cationic degree is 90%.
embodiment 4:uV-light causes a synthetic method for dewatered modified cation polyacrylamide, it is characterized in that, comprises the following steps:
The first step, deionized water 91.8ml is added successively in reaction unit, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (DMC) 0.5g, Butyl Acrylate Monomer (BA) 0.2g and acrylamide monomer (AM) 9.5g stirs to dissolving formation monomer solution completely, wherein deionized water is as solvent, meter MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride monomer (DMC), Butyl Acrylate Monomer (BA) and acrylamide monomer (AM) are total monomer, meter MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (DMC) and acrylamide monomer (AM) are total water-soluble monomer, in monomer solution, total monomer quality mark is 10%, and the mass percent of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride monomer and acrylamide monomer is 5%:95%, and Butyl Acrylate Monomer accounts for 2.0% of total water-soluble mono weight,
Second step, in above-mentioned monomer solution, add account for total water-soluble mono weight 0.2.% urea as solubility promoter, add account for total water-soluble mono weight 1.0% cetyl trimethylammonium bromide (CTAB) as tensio-active agent, add account for total water-soluble mono weight 0.1 ‰ azo two isobutyl imidazoline hydrochloride VA-044 as initiator, be uniformly mixed, then add mineral acid and the pH value of monomer solution is adjusted to 2. by mineral alkali; Then be filled with High Purity Nitrogen to reaction unit, after the air in reaction unit is got rid of completely, reaction unit sealed;
3rd step, under Interior Temperature Environment, reaction unit after sealing in second step is put into UV-light reaction unit, initiated polymerization is carried out under UV-irradiation, wavelength 200nm ~ the 400nm sent by high voltage mercury lamp during this UV-light, the UV-light of predominant wavelength 365nm, takes out after 20min, leave standstill slaking more than 1 hour, obtained gluey dewatered modified cation polyacrylamide;
4th step, particulate state made by the gluey dewatered modified cation polyacrylamide 3rd step obtained, long-pending ratio is used to be that the dehydrated alcohol of 2:1 and the mixing solutions of acetone are purified for three times, wash, refined, then grinding after drying in vacuum drying oven, obtains dewatered modified cation Polyacrylamide Powder.
Employing colloid titration method detects, and the limiting viscosity recording the dewatered modified cation polyacrylamide finally obtained is 1937.2 mL/g, and solid content is 31.2%, and cationic degree is 5%.
embodiment 5:uV-light causes a synthetic method for dewatered modified cation polyacrylamide, it is characterized in that, comprises the following steps:
The first step, deionized water 32.4ml is added successively in reaction unit, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (DMC) 2.0g, Butyl Acrylate Monomer (BA) 0.8g and acrylamide monomer (AM) 8.0g stirs to dissolving formation monomer solution completely, wherein deionized water is as solvent, meter MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride monomer (DMC), Butyl Acrylate Monomer (BA) and acrylamide monomer (AM) are total monomer, meter MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (DMC) and acrylamide monomer (AM) are total water-soluble monomer, in monomer solution, total monomer quality mark is 25%, and the mass percent of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride monomer and acrylamide monomer is 20%:80%, and Butyl Acrylate Monomer accounts for 8.0% of total water-soluble mono weight,
Second step, in above-mentioned monomer solution, add account for total water-soluble mono weight 1.0.% urea as solubility promoter, add account for total water-soluble mono weight 2.0% cetyl trimethylammonium bromide (CTAB) as tensio-active agent, add the composite initiator accounting for total water-soluble mono weight 0.5 ‰, in this composite initiator ammonium persulphate, sodium bisulfite and azo two the mass ratio of isobutyl imidazoline hydrochloride VA-044 be 4:1:1, be uniformly mixed, then add mineral acid and the pH value of monomer solution is adjusted to 5. by mineral alkali; Then be filled with High Purity Nitrogen to reaction unit, after the air in reaction unit is got rid of completely, reaction unit sealed;
3rd step, under Interior Temperature Environment, reaction unit after sealing in second step is put into UV-light reaction unit, initiated polymerization is carried out under UV-irradiation, wavelength 200nm ~ the 400nm sent by high voltage mercury lamp during this UV-light, the UV-light of predominant wavelength 365nm, takes out after 60min, leave standstill slaking more than 1 hour, obtained gluey dewatered modified cation polyacrylamide;
4th step, particulate state made by the gluey dewatered modified cation polyacrylamide 3rd step obtained, long-pending ratio is used to be that the dehydrated alcohol of 2:1 and the mixing solutions of acetone are purified for three times, wash, refined, then grinding after drying in vacuum drying oven, obtains dewatered modified cation Polyacrylamide Powder.
Employing colloid titration method detects, and the limiting viscosity recording the dewatered modified cation polyacrylamide finally obtained is 1579.5mL/g, and solid content is 35.3%, and cationic degree is 20%.
embodiment 6:uV-light causes a synthetic method for dewatered modified cation polyacrylamide, it is characterized in that, comprises the following steps:
The first step, deionized water 11.0ml is added successively in reaction unit, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (DMC) 9.0g, Butyl Acrylate Monomer (BA) 1.0g and acrylamide monomer (AM) 1.0g stirs to dissolving formation monomer solution completely, wherein deionized water is as solvent, meter MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride monomer (DMC), Butyl Acrylate Monomer (BA) and acrylamide monomer (AM) are total monomer, meter MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride (DMC) and acrylamide monomer (AM) are total water-soluble monomer, in monomer solution, total monomer quality mark is 50%, and the mass percent of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride monomer and acrylamide monomer is 90%:10%, and Butyl Acrylate Monomer accounts for 10% of total water-soluble mono weight,
Second step, in above-mentioned monomer solution, add account for total water-soluble mono weight 2.0.% urea as solubility promoter, add account for total water-soluble mono weight 6.0% cetyl trimethylammonium bromide (CTAB) as tensio-active agent, add account for total water-soluble mono weight 0.8 ‰ azo two isobutyl imidazoline hydrochloride VA-044 as initiator, be uniformly mixed, then add mineral acid and the pH value of monomer solution is adjusted to 6 by mineral alkali; Then be filled with High Purity Nitrogen to reaction unit, after the air in reaction unit is got rid of completely, reaction unit sealed;
3rd step, under Interior Temperature Environment, reaction unit after sealing in second step is put into UV-light reaction unit, initiated polymerization is carried out under UV-irradiation, wavelength 200nm ~ the 400nm sent by high voltage mercury lamp during this UV-light, the UV-light of predominant wavelength 365nm, takes out after 80min, leave standstill slaking more than 1 hour, obtained gluey dewatered modified cation polyacrylamide;
4th step, particulate state made by the gluey dewatered modified cation polyacrylamide 3rd step obtained, long-pending ratio is used to be that the dehydrated alcohol of 2:1 and the mixing solutions of acetone are purified for three times, wash, refined, then grinding after drying in vacuum drying oven, obtains dewatered modified cation Polyacrylamide Powder.
Employing colloid titration method detects, and the limiting viscosity recording the dewatered modified cation polyacrylamide finally obtained is 692.6mL/g, and solid content is 27.1%, and cationic degree is 90%.
embodiment 7:uV-light causes a synthetic method for dewatered modified cation polyacrylamide, it is characterized in that, comprises the following steps:
The first step, deionized water 15.6ml is added successively in reaction unit, acrylyl oxy-ethyl-trimethyl salmiac monomer (DAC) 4.0g, Butyl Acrylate Monomer (BA) 0.4g and acrylamide monomer (AM) 6.0g stirs to dissolving formation monomer solution completely, wherein deionized water is as solvent, meter acrylyl oxy-ethyl-trimethyl salmiac monomer (DAC), Butyl Acrylate Monomer (BA) and acrylamide monomer (AM) are total monomer, meter acrylyl oxy-ethyl-trimethyl salmiac monomer (DAC) and acrylamide monomer (AM) are total water-soluble monomer, in monomer solution, total monomer quality mark is 50%, and the mass percent of acrylyl oxy-ethyl-trimethyl salmiac monomer and acrylamide monomer is 40%:60%, and Butyl Acrylate Monomer accounts for 4.0% of total water-soluble mono weight,
Second step, in above-mentioned monomer solution, add account for total water-soluble mono weight 1.3.% urea as solubility promoter, add account for total water-soluble mono weight 3.0% cetyl trimethylammonium bromide (CTAB) as tensio-active agent, add account for total water-soluble mono weight 0.6 ‰ azo two isobutyl imidazoline hydrochloride VA-044 as initiator, be uniformly mixed, then add mineral acid and the pH value of monomer solution is adjusted to 3 by mineral alkali; Then be filled with High Purity Nitrogen to reaction unit, after the air in reaction unit is got rid of completely, reaction unit sealed;
3rd step, under Interior Temperature Environment, reaction unit after sealing in second step is put into UV-light reaction unit, initiated polymerization is carried out under UV-irradiation, wavelength 200nm ~ the 400nm sent by high voltage mercury lamp during this UV-light, the UV-light of predominant wavelength 365nm, takes out after 65min, leave standstill slaking more than 1 hour, obtained gluey dewatered modified cation polyacrylamide;
4th step, particulate state made by the gluey dewatered modified cation polyacrylamide 3rd step obtained, long-pending ratio is used to be that the dehydrated alcohol of 2:1 and the mixing solutions of acetone are purified for three times, wash, refined, then grinding after drying in vacuum drying oven, obtains dewatered modified cation Polyacrylamide Powder.
Employing colloid titration method detects, and the limiting viscosity recording the dewatered modified cation polyacrylamide finally obtained is 1894.8 mL/g, and solid content is 32.4 %, and cationic degree is 40 %.
embodiment 8:uV-light causes a synthetic method for dewatered modified cation polyacrylamide, it is characterized in that, comprises the following steps:
The first step, deionized water 13.0ml is added successively in reaction unit, acrylyl oxy-ethyl-trimethyl salmiac monomer (DAC) 2.0g, Butyl Acrylate Monomer (BA) 1.6g and acrylamide monomer (AM) 8.0g stirs to dissolving formation monomer solution completely, wherein deionized water is as solvent, meter acrylyl oxy-ethyl-trimethyl salmiac monomer (DAC), Butyl Acrylate Monomer (BA) and acrylamide monomer (AM) are total monomer, meter acrylyl oxy-ethyl-trimethyl salmiac monomer (DAC) and acrylamide monomer (AM) are total water-soluble monomer, in monomer solution, total monomer quality mark is 45%, and the mass percent of acrylyl oxy-ethyl-trimethyl salmiac monomer and acrylamide monomer is 20%:80%, and Butyl Acrylate Monomer accounts for 6.0% of total water-soluble mono weight,
Second step, in above-mentioned monomer solution, add account for total water-soluble mono weight 0.8.% urea as solubility promoter, add account for total water-soluble mono weight 3.0% cetyl trimethylammonium bromide (CTAB) as tensio-active agent, add account for total water-soluble mono weight 0.6 ‰ azo two isobutyl imidazoline hydrochloride VA-044 as initiator, be uniformly mixed, then add mineral acid and the pH value of monomer solution is adjusted to 5 by mineral alkali; Then be filled with High Purity Nitrogen to reaction unit, after the air in reaction unit is got rid of completely, reaction unit sealed;
3rd step, under Interior Temperature Environment, reaction unit after sealing in second step is put into UV-light reaction unit, initiated polymerization is carried out under UV-irradiation, wavelength 200nm ~ the 400nm sent by high voltage mercury lamp during this UV-light, the UV-light of predominant wavelength 365nm, takes out after 55min, leave standstill slaking more than 1 hour, obtained gluey dewatered modified cation polyacrylamide;
4th step, particulate state made by the gluey dewatered modified cation polyacrylamide 3rd step obtained, long-pending ratio is used to be that the dehydrated alcohol of 2:1 and the mixing solutions of acetone are purified for three times, wash, refined, then grinding after drying in vacuum drying oven, obtains dewatered modified cation Polyacrylamide Powder.
Employing colloid titration method detects, and the limiting viscosity recording the dewatered modified cation polyacrylamide finally obtained is 1953.1 mL/g, and solid content is 33.1%, and cationic degree is 20 %.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (4)
1. UV-light causes a synthetic method for dewatered modified cation polyacrylamide, it is characterized in that, comprises the following steps:
The first step, deionized water, cationic monomer is added successively in reaction unit, hydrophobic monomer and acrylamide monomer stir to dissolving formation monomer solution completely, wherein deionized water is as solvent, meter cationic monomer, hydrophobic monomer and acrylamide monomer are total monomer, and meter cationic monomer and acrylamide monomer are total water-soluble monomer; In described monomer solution, total monomer quality mark is 10% ~ 50%, and the mass percent of described cationic monomer and acrylamide monomer is 5% ~ 90%:10% ~ 95%, and described hydrophobic monomer accounts for 2.0% ~ 10% of total water-soluble mono weight;
Described cationic monomer is acrylyl oxy-ethyl-trimethyl salmiac or MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride;
Described hydrophobic monomer is butyl acrylate, octadecyl acrylate or dimethylaminoethyl methacrylate;
Second step, in above-mentioned monomer solution, add account for total water-soluble mono weight 0.2% ~ 2% urea as solubility promoter, add account for total water-soluble mono weight 1% ~ 6% cetyl trimethylammonium bromide as tensio-active agent, add the initiator accounting for total water-soluble mono weight 0.1 ‰ ~ 0.8 ‰, be uniformly mixed, then add mineral acid and the pH value of monomer solution is adjusted to 2. ~ 6 by mineral alkali; Then be filled with High Purity Nitrogen to reaction unit, after the air in reaction unit is got rid of completely, reaction unit sealed;
3rd step, under Interior Temperature Environment, puts into UV-light reaction unit by the reaction unit after sealing in second step, initiated polymerization is carried out under UV-irradiation, take out after 20min ~ 80min, leave standstill slaking more than 1 hour, obtained gluey dewatered modified cation polyacrylamide;
4th step, particulate state made by the gluey dewatered modified cation polyacrylamide 3rd step obtained, long-pending ratio is used to be that the dehydrated alcohol of 2:1 and the mixed solutions for many times of acetone are purified, wash, refined, then grinding after drying in vacuum drying oven, obtains dewatered modified cation Polyacrylamide Powder.
2. UV-light causes the synthetic method of dewatered modified cation polyacrylamide according to claim 1, and it is characterized in that, the initiator in described second step is azo-bis-isobutyrate hydrochloride V-50 or azo two isobutyl imidazoline hydrochloride VA-044.
3. UV-light according to claim 1 causes the synthetic method of dewatered modified cation polyacrylamide, it is characterized in that, initiator in described second step is composite initiator, this composite initiator is made up of organic initiators and inorganic initiator, wherein organic initiators is azo-bis-isobutyrate hydrochloride V-50 or azo two isobutyl imidazoline hydrochloride VA-044, and inorganic initiator is ammonium persulphate and sodium bisulfite; The mass ratio of described ammonium persulphate, organic initiators and sodium bisulfite is (2 ~ 4): (1 ~ 2): (1 ~ 2).
4. the UV-light according to any one of claim 1-3 causes the synthetic method of dewatered modified cation polyacrylamide, it is characterized in that, in described second step UV-light produced by high voltage mercury lamp, and the ultraviolet wavelength produced is 200nm ~ 400nm, predominant wavelength is 365nm, and light intensity is 600 ~ 1800 uw/cm
2.
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| CN107325213B (en) * | 2017-08-09 | 2019-09-10 | 江苏富淼科技股份有限公司 | A kind of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride method for producing polymer of adjustable molecular weight section |
| CN107573448A (en) * | 2017-09-13 | 2018-01-12 | 重庆大学 | A kind of method for triggering Syn-Organic flocculants using ultraviolet light and hydrogen peroxide system |
| CN109293808B (en) * | 2018-10-26 | 2021-01-01 | 江门市新会区中盛生物科技有限公司 | Preparation method of water-soluble acidic sodium polyacrylate |
| CN109575185A (en) * | 2018-12-25 | 2019-04-05 | 上海纳米技术及应用国家工程研究中心有限公司 | The preparation of fluorided-modified hydrophobicity amphoteric organic polymer coargulator and product and application |
| CN111499798A (en) * | 2020-04-28 | 2020-08-07 | 广东轻工职业技术学院 | Preparation method of hydrophobically associating cationic polyacrylamide and sludge dewatering application |
| CN111995026B (en) * | 2020-06-28 | 2022-06-21 | 赖继平 | Environment-friendly efficient composite biological flocculant and preparation method thereof |
| CN114409846A (en) * | 2022-02-28 | 2022-04-29 | 南京瑞迪高新技术有限公司 | Synthesis method of photopolymerized hydrophobically modified polyacrylamide |
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