CN101157736A - Method for preparing high molecular weight anion type polyacrylamide by ultralow-temperature initiation - Google Patents
Method for preparing high molecular weight anion type polyacrylamide by ultralow-temperature initiation Download PDFInfo
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Abstract
The present invention provides a preparation method of anionic polyacrylamide with a high molecular weight by ultra-low-temperature initiation, a polynary initiator and a plurality of additives are added in the acrylamide water solution, and high-purity nitrogen is introduced for water solution polymerization. The colloids are carried out the hydrolysis by granulation, adding the hydrolytic agents, mixing and heating after a period of polymerization and aging, after that, the anionic polyacrylamide with a molecular weight of more than 25 million can be generated by granulation, drying, smashing and screening, the present invention has the advantages of smooth polymerization reaction, being conductive to the growth of a chain and the formation of the products with the high molecular weight, overcoming the shortcoming of slow temperature increase or uneven speed of temperature increase of a single azo initiator, low initiation temperature and so on.
Description
Technical field:
The invention belongs to the chemical synthesis process of water-soluble polyacrylamide polymkeric substance, particularly relate to a kind of method for preparing the ultra high molecular weight anion-type polyacrylamide of relative molecular mass more than 2,500 ten thousand.
Background technology:
The high molecular anion type polycrylamide industrial production is comparative maturity, but it is also relatively more difficult that the Industrial products molecular weight is stabilized in more than 2,500 ten thousand.At present domestic and international anionic polyacrylamide gets production technique and mainly is divided into preceding hydrolysis and two kinds of methods of posthydrolysis: preceding hydrolysis adds hydrolytic reagents such as yellow soda ash, sodium bicarbonate or sodium hydroxide exactly in acrylamide solution, add various auxiliary agents such as initiator after the logical nitrogen deoxygenation and carry out aqueous solution polymerization, the post-heating hydrolysis is finished in polymerization, produce the method for polyacrylamide again through granulation, drying, pulverizing, screening, as open among the CN1168894.Advantages such as it is simple that this method has technology, and facility investment is less.But no matter use which kind of initiator system, adopt the sort of initiation mode, preceding hydrolysis all is difficult to obtain high molecular weight polyacrylamide, and general molecular weight is less than 1,700 ten thousand.Posthydrolysis is exactly to add various auxiliary agents such as initiator and carries out polymerization in acrylamide solution, after aging for some time of polymerization colloid added hydrolytic reagent Hybrid Heating such as sodium hydroxide through granulation and be hydrolyzed, produce the method for polyacrylamide afterwards again through granulation, drying, pulverizing, screening.As open among the CN1057059A.Though this method can be produced the higher molecular weight anion-type polyacrylamide, molecular weight also is difficult to surpass 2,000 ten thousand.
Summary of the invention
The objective of the invention is to avoid the deficiency of above-mentioned technology, and a kind of method of preparing high molecular weight anion type polyacrylamide by ultralow-temperature initiation is provided.
The object of the present invention is achieved like this: add polynary initiator, various auxiliary agent in acrylamide solution, and the feeding high pure nitrogen carries out aqueous solution polymerization.After aging for some time of polymerization colloid is added the hydrolytic reagent Hybrid Heating through granulation and be hydrolyzed, produce molecular weight through granulation, drying, pulverizing, screening more afterwards and surpass 2,500 ten thousand anionic polyacrylamide.
Purpose of the present invention can also realize like this:
A kind of method of preparing high molecular weight anion type polyacrylamide by ultralow-temperature initiation, hydrolytic reagent are solid sodium hydroxide, the weight percent 10-20% of add-on, and add-on can be by the degree of hydrolysis adjustment of polypropylene phthalein amine.Polynary initiator is made up of oxygenant, reductive agent, multiple water-soluble azo class initiator, and oxygenant is a persulphate, and as Potassium Persulphate, Sodium Persulfate, ammonium persulphate, add-on is the 0.0001-0.5% to the acrylamide monomer solution weight; Reductive agent is a sulphite, and as S-WAT, ammonium sulphite, potassium sulfite, sodium bisulfite, Sodium Metabisulfite, potassium metabisulfite, add-on is the 0.0005-0.25% to the acrylamide monomer solution weight; Water-soluble azo class initiator is 2,2 '-azo (2-amidine propane) dihydrochloride, 2,2 '-azo [2-(2-tetrahydroglyoxaline-2-yl) propane] dihydrochloride, 2,2 '-azo [2-methyl-N-(2-methacrylic acid) propionic acid amide], add-on is the 0.001-0.5% to the acrylamide monomer solution weight.The weight ratio of three kinds of azo initiators is 4: 4: 2.Auxiliary agent urea add-on is the 0.10-0.50% to the acrylamide monomer solution weight, the ammoniacal liquor add-on is the 0.005-0.20% to the acrylamide monomer solution weight, and the disodium ethylene diamine tetraacetate add-on is the 0.005-0.05% to the acrylamide monomer solution weight.
Acrylamide solution concentration among the present invention is controlled at 15-35%, and kick off temperature is 0-5 ℃, and the adiabatic polymerisation time is 1-5h.Aging 1-3h after adiabatic polymerisation is finished adds sodium hydrate solid after the preliminary granulation and mixes, and heat temperature raising to hydrolysis temperature is 85-105 ℃, and hydrolysis time is 2-6h., obtain molecular weight greater than 2,500 ten thousand anion-polyacrylamide through granulation, oven dry, pulverizing, screening.
Compared with prior art, advantage of the present invention is:
1, the initiator system that adopts redox to cooperate with multiple azo initiator, stable polymerization reaction helps the growth of chain, forms high molecular weight products;
2, use uses that proportion of multiple azo initiator in the initiator, overcome single azo initiator and heated up slowly or the uneven shortcoming of heat-up rate, improved the overall performance of initiator system;
3, kick off temperature is low, helps the raising of molecular weight product.
Embodiment
Further specify embodiments of the invention below by embodiment.
Embodiment 1
In 15 cubic metres strap clamp cover refrigerative batching still, stir the acrylamide 6600kg of adding 30% down, pure water 2200kg, urea 5kg, ammoniacal liquor 6kg, disodium ethylene diamine tetraacetate 400g, 2,2 '-azo (2-amidine propane) dihydrochloride 320g, 2,2 '-azo [2-(2-tetrahydroglyoxaline-2-yl) propane] dihydrochloride 320g, 2,2 '-azo [2-methyl-N-(2-methacrylic acid) propionic acid amide] 160g feeds-10 ℃ of refrigerated water coolings in chuck, adjust 3 ℃ of kick off temperatures.The acrylamide soln for preparing is put into polymeric kettle, feed high pure nitrogen to remove dissolved oxygen in the reaction system, add ammonium persulphate 120g behind the logical nitrogen 30min, behind the 5min, add sodium bisulfite 90g, continue to stop nitrogen behind the logical nitrogen 15min, material begins to heat up in the still, 2.5h back temperature in the kettle reaches 71.3 ℃, wears out and carries out granulation after 1 hour, the polyacrylamide after the granulation is put into the hydrolyzer of 85 ℃ of chuck heating, stir and add solid sodium hydroxide 320kg down, keep 85 ℃ of hydrolysis 4h after stirring, pass through granulation afterwards, dry, pulverize, screening obtains molecular weight 2,694 ten thousand, the high molecular weight anionic polyacrylamide amine product of degree of hydrolysis 24.1%.
Embodiment 2
In 15 cubic metres strap clamp cover refrigerative batching still, stir the acrylamide 6600kg of adding 30% down, pure water 2200kg,, 5kg urea, ammoniacal liquor 6kg, disodium ethylene diamine tetraacetate 200g, 2,2 '-azo (2-amidine propane) dihydrochloride 300g, 2,2 '-azo [2-(2-tetrahydroglyoxaline-2-yl) propane] dihydrochloride 300g, 2,2 '-azo [2-methyl-N-(2-methacrylic acid) propionic acid amide] 150g feeds-10 ℃ of refrigerated water coolings in chuck, adjust 5 ℃ of kick off temperatures.The acrylamide soln for preparing is put into polymeric kettle, feed high pure nitrogen to remove dissolved oxygen in the reaction system, add ammonium persulphate 150g behind the logical nitrogen 30min, behind the 5min, add S-WAT 120g, continue to stop nitrogen behind the logical nitrogen 15min, material begins to heat up in the still, temperature in the kettle reaches 73.2 ℃ behind the 2h, wears out and carries out granulation after 1 hour, the polyacrylamide after the granulation is put into the hydrolyzer of 85 ℃ of chuck heating, stir and add solid sodium hydroxide 290kg down, keep 85 ℃ of hydrolysis 4h after stirring, pass through granulation afterwards, dry, pulverize, screening obtains molecular weight 2,587 ten thousand, the high molecular weight anionic polyacrylamide amine product of degree of hydrolysis 22.5%.
Embodiment 3
In 15 cubic metres strap clamp cover refrigerative batching still, stir the acrylamide monomer 6600kg of adding 30% down, deionized water (electricity is led≤2.0 μ s/cm) 2200kg,, urea 5kg, ammoniacal liquor (content 25-28%) 6kg, disodium ethylene diamine tetraacetate 200g, 2,2 '-azo (2-amidine propane) dihydrochloride 300g, 2,2 '-azo [2-(2-tetrahydroglyoxaline-2-yl) propane] dihydrochloride 300g, 2,2 '-azo [2-methyl-N-(2-methacrylic acid) propionic acid amide] 150g, in chuck, feed-10 ℃ of refrigerated water coolings, adjust 1.5 ℃ of kick off temperatures.The acrylamide soln for preparing is put into polymeric kettle, feed high pure nitrogen (purity 〉=99.999%) to remove dissolved oxygen in the reaction system, nitrogen flow 〉=80m
3/ h adds Potassium Persulphate 96g behind the logical nitrogen 30min, behind the 5min, adds sodium bisulfite 96g, continues to stop nitrogen behind the logical nitrogen 15min, and material begins to heat up in the still, and temperature in the kettle reaches 70.8 ℃ of top temperatures behind the 3h.Polymerization is finished to wear out and is carried out granulation after 1 hour, polyacrylamide after the granulation is put into the hydrolyzer of 85 ℃ of chuck heating, stir and add solid sodium hydroxide 380kg down, 85 ℃ of hydrolysis 4h of back maintenance stir, obtain molecular weight 2,783 ten thousand, the high molecular weight anionic polyacrylamide amine product of degree of hydrolysis 28.9% through granulation, drying, pulverizing, screening afterwards.
From the foregoing description as can be seen, can produce molecular weight according to the present invention greater than 2,500 ten thousand polyacrylamide Industrial products.
Claims (8)
1. the method for a preparing high molecular weight anion type polyacrylamide by ultralow-temperature initiation, employing very low temperature causes, adiabatic polymerisation, the posthydrolysis mode, it is characterized in that: adding weight concentration in polymeric kettle is the 15-35% acrylamide monomer aqueous solution, initiator, auxiliary agent, feeds nitrogen flooding oxygen and carries out adiabatic polymerisation, adds alkali and be hydrolyzed after preliminary granulation, carry out granulation, oven dry behind the hydrolysis certain hour, pulverize, sieve, obtain final product.
2. the method for a kind of preparing high molecular weight anion type polyacrylamide by ultralow-temperature initiation according to claim 1, it is characterized in that: the present invention adopts initiator to make the polynary initiator system that oxidation-reduction trigger system that oxygenant and sulphite or hydrosulphite form as reductive agent and multiple water-soluble azo class initiator are formed by persulphate, wherein the add-on of oxygenant is the 0.0001-0.5% of acrylamide monomer aqueous solution weight, reductive agent is the 0.0001-0.25% of acrylamide monomer aqueous solution weight, and azo-initiator is the 0.001-0.50% of acrylamide monomer aqueous solution weight.
3. the method for a kind of preparing high molecular weight anion type polyacrylamide by ultralow-temperature initiation according to claim 1, it is characterized in that: preferred oxidant is Potassium Persulphate or Sodium Persulfate or ammonium persulphate, and add-on is the 0.0001-0.5% of acrylamide monomer aqueous solution weight; Reductive agent is a sulphite, and as S-WAT, ammonium sulphite, potassium sulfite, sodium bisulfite, Sodium Metabisulfite or potassium metabisulfite, add-on is the 0.0005-0.25% to acrylamide monomer aqueous solution weight; Water-soluble azo class initiator is 2,2 '-azo (2-amidine propane) dihydrochloride, 2,2 '-azo [2-(2-tetrahydroglyoxaline-2-yl) propane] dihydrochloride and 2,2 '-azo [2-methyl-N-(2-methacrylic acid) propionic acid amide], add-on is the 0.001-0.5% of acrylamide monomer aqueous solution weight.
4. the method for a kind of preparing high molecular weight anion type polyacrylamide by ultralow-temperature initiation according to claim 1, it is characterized in that: water-soluble azo initiator adds by a certain percentage, 2,2 '-azo (2-amidine propane) dihydrochloride, 2,2 '-azo [2-(2-tetrahydroglyoxaline-2-yl) propane] dihydrochloride, 2, the weight ratio of three kinds of azo initiators of 2 '-azo [2-methyl-N-(2-methacrylic acid) propionic acid amide] is 4: 4: 2.
5. the method for a kind of preparing high molecular weight anion type polyacrylamide by ultralow-temperature initiation according to claim 1, it is characterized in that: outer adding assistant is urea, ammoniacal liquor and disodium ethylene diamine tetraacetate, the urea add-on is the 0.10-0.50% of acrylamide monomer aqueous solution weight, the ammoniacal liquor add-on is the 0.005-0.20% of acrylamide monomer aqueous solution weight, and the disodium ethylene diamine tetraacetate add-on is the 0.005-0.05% of acrylamide monomer aqueous solution weight.
6. the method for a kind of preparing high molecular weight anion type polyacrylamide by ultralow-temperature initiation according to claim 1, it is characterized in that: kick off temperature is 0-5 ℃,
7. the method for a kind of preparing high molecular weight anion type polyacrylamide by ultralow-temperature initiation according to claim 1, it is characterized in that: kick off temperature is preferably 1-3 ℃.
8. the method for a kind of preparing high molecular weight anion type polyacrylamide by ultralow-temperature initiation according to claim 1, it is characterized in that: hydrolytic reagent is a solid sodium hydroxide, the weight percent 10-20% of add-on.Hydrolysis temperature is 85-105 ℃, and hydrolysis time is 2-6h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102050914A (en) * | 2009-10-27 | 2011-05-11 | 中国石油化工股份有限公司 | Ultra-high molecular weight sulfonic acid type acrylamide and preparation method thereof |
| CN103087236A (en) * | 2013-02-04 | 2013-05-08 | 东营顺通化工（集团）有限公司 | Method for preparing high-molecular-weight anionic polyacrylamide through ultralow-temperature initiation |
| CN103113517A (en) * | 2013-02-04 | 2013-05-22 | 东营顺通化工（集团）有限公司 | Synthesis method of high molecular weight temperature and salt resistant polyacrylamide |
| CN103304714A (en) * | 2013-06-26 | 2013-09-18 | 上海宇昂水性新材料科技股份有限公司 | Preparation method of instant ultra-high molecular weight polyacrylamide dry powder |
| CN103509154A (en) * | 2012-06-28 | 2014-01-15 | 中国石油化工股份有限公司 | Preparation method of zwitterionic polyacrylamide |
| CN103509146A (en) * | 2012-06-27 | 2014-01-15 | 中国石油化工股份有限公司 | Preparation method of ultra-high molecular weight anionic polyacrylamide |
| CN103709287A (en) * | 2013-12-04 | 2014-04-09 | 天津大港油田滨港集团博弘石油化工有限公司 | Preparation method for polyacrylamide with salt resistance and high viscosity |
| CN103739758A (en) * | 2014-01-09 | 2014-04-23 | 安徽天润化学工业股份有限公司 | Preparation method of polyacrylamide for oil field |
| CN103739775A (en) * | 2013-12-04 | 2014-04-23 | 天津大港油田滨港集团博弘石油化工有限公司 | Preparation method of salt-tolerant high-temperature resistant polyacrylamide |
| CN104231138A (en) * | 2014-08-19 | 2014-12-24 | 杭州电子科技大学 | Preparation method of polyacrylamide high-polymer moisture absorption material |
| CN104262517A (en) * | 2014-10-23 | 2015-01-07 | 山东宝莫生物化工股份有限公司 | Continuous posthydrolysis method for polyacrylamide |
| CN104371054A (en) * | 2014-11-07 | 2015-02-25 | 安徽天润化学工业股份有限公司 | Preparation method of high-molecular-weight anionic polyacrylamide |
| CN105348439A (en) * | 2015-11-20 | 2016-02-24 | 中国海洋石油总公司 | Preparation method of high-solid-content polyacrylamide emulsion |
| CN110294820A (en) * | 2018-03-21 | 2019-10-01 | 上海四奥化工有限公司 | A kind of preparation method of super high molecular weight polyacrylamide |
| CN114196109A (en) * | 2021-12-08 | 2022-03-18 | 武汉金发科技有限公司 | Polypropylene odor adsorption master batch and preparation method thereof |
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- 2007-09-28 CN CNA2007101129927A patent/CN101157736A/en active Pending
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| CN102050914A (en) * | 2009-10-27 | 2011-05-11 | 中国石油化工股份有限公司 | Ultra-high molecular weight sulfonic acid type acrylamide and preparation method thereof |
| CN102050914B (en) * | 2009-10-27 | 2012-11-21 | 中国石油化工股份有限公司 | Ultra-high molecular weight sulfonic acid type acrylamide and preparation method thereof |
| CN103509146B (en) * | 2012-06-27 | 2016-04-13 | 中国石油化工股份有限公司 | The preparation method of ultra high molecular weight anion-type polyacrylamide |
| CN103509146A (en) * | 2012-06-27 | 2014-01-15 | 中国石油化工股份有限公司 | Preparation method of ultra-high molecular weight anionic polyacrylamide |
| CN103509154A (en) * | 2012-06-28 | 2014-01-15 | 中国石油化工股份有限公司 | Preparation method of zwitterionic polyacrylamide |
| CN103509154B (en) * | 2012-06-28 | 2017-02-01 | 中国石油化工股份有限公司 | Preparation method of zwitterionic polyacrylamide |
| CN103113517A (en) * | 2013-02-04 | 2013-05-22 | 东营顺通化工（集团）有限公司 | Synthesis method of high molecular weight temperature and salt resistant polyacrylamide |
| CN103087236A (en) * | 2013-02-04 | 2013-05-08 | 东营顺通化工（集团）有限公司 | Method for preparing high-molecular-weight anionic polyacrylamide through ultralow-temperature initiation |
| CN103304714A (en) * | 2013-06-26 | 2013-09-18 | 上海宇昂水性新材料科技股份有限公司 | Preparation method of instant ultra-high molecular weight polyacrylamide dry powder |
| CN103739775A (en) * | 2013-12-04 | 2014-04-23 | 天津大港油田滨港集团博弘石油化工有限公司 | Preparation method of salt-tolerant high-temperature resistant polyacrylamide |
| CN103739775B (en) * | 2013-12-04 | 2015-10-28 | 天津大港油田滨港集团博弘石油化工有限公司 | A kind of preparation method of salt-tolerant high-temperature resistant polyacrylamide |
| CN103709287A (en) * | 2013-12-04 | 2014-04-09 | 天津大港油田滨港集团博弘石油化工有限公司 | Preparation method for polyacrylamide with salt resistance and high viscosity |
| CN103739758A (en) * | 2014-01-09 | 2014-04-23 | 安徽天润化学工业股份有限公司 | Preparation method of polyacrylamide for oil field |
| CN104231138A (en) * | 2014-08-19 | 2014-12-24 | 杭州电子科技大学 | Preparation method of polyacrylamide high-polymer moisture absorption material |
| CN104231138B (en) * | 2014-08-19 | 2017-06-06 | 杭州电子科技大学 | A kind of preparation method of polyacrylamide polymer absorbent material |
| CN104262517A (en) * | 2014-10-23 | 2015-01-07 | 山东宝莫生物化工股份有限公司 | Continuous posthydrolysis method for polyacrylamide |
| CN104262517B (en) * | 2014-10-23 | 2016-12-07 | 山东宝莫生物化工股份有限公司 | Method for hydrolysis after a kind of polyacrylamide serialization |
| CN104371054A (en) * | 2014-11-07 | 2015-02-25 | 安徽天润化学工业股份有限公司 | Preparation method of high-molecular-weight anionic polyacrylamide |
| CN105348439A (en) * | 2015-11-20 | 2016-02-24 | 中国海洋石油总公司 | Preparation method of high-solid-content polyacrylamide emulsion |
| CN110294820A (en) * | 2018-03-21 | 2019-10-01 | 上海四奥化工有限公司 | A kind of preparation method of super high molecular weight polyacrylamide |
| CN110294820B (en) * | 2018-03-21 | 2022-06-24 | 上海四奥化工有限公司 | Preparation method of polyacrylamide with ultrahigh molecular weight |
| CN114196109A (en) * | 2021-12-08 | 2022-03-18 | 武汉金发科技有限公司 | Polypropylene odor adsorption master batch and preparation method thereof |
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