CN101591415A - Iso-hydroxamic modified polyacrylamide and preparation method thereof - Google Patents
Iso-hydroxamic modified polyacrylamide and preparation method thereof Download PDFInfo
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- CN101591415A CN101591415A CNA2009100631510A CN200910063151A CN101591415A CN 101591415 A CN101591415 A CN 101591415A CN A2009100631510 A CNA2009100631510 A CN A2009100631510A CN 200910063151 A CN200910063151 A CN 200910063151A CN 101591415 A CN101591415 A CN 101591415A
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Abstract
The present invention relates to the high molecular synthesis technique of a kind of water-solubility function, particularly adopt the method for reversed-phase emulsion copolymerization, synthesize the supra polymer modified polyacrylamide in fields such as satisfying mineral selecting and purchasing, oil recovery and city domestic sewage processing.Belong to fine chemistry industry, also belong to the Polymer Synthesizing field simultaneously.Its product dissolution time is short, gel-free body and insoluble micelle, and the molecular weight height is specially adapted to refine the red-mud settlement flocculation in the alumina technology process from bauxite.
Description
Technical field
The present invention relates to the high molecular synthesis technique of a kind of water-solubility function, particularly adopt the method for reversed-phase emulsion copolymerization, synthesize the modified polyacrylamide of the supra polymer in fields such as satisfying mineral selecting and purchasing, oil recovery and city domestic sewage processing.Belong to fine chemistry industry, also belong to the Polymer Synthesizing field simultaneously.
Background technology
Polyacrylamide (PAM) is a kind of water-solubility function Molecularly Imprinted Polymer of line style, is one of most widely used kind in the water-soluble polymer.Have application widely in industries such as oil production, water treatment, weaving, printing and dyeing, papermaking, ore dressing, coal washing, medicine, sugaring, breed, building materials, agriculturals, " all trades auxiliary agent ", " title of omnipotent product " are arranged.
Polyacrylamide is mainly with the commodity selling of two kinds of forms, and a kind of is Powdered, and another kind is a colloid.Colloid is difficult for transportation, uses also inconvenient.The powdered polypropylene acid amides is more popular with users, but also has shortcomings such as dissolution time length, equipment input and labour intensity are big.Occurred polymeric dispersions recently, be called polyacrylamide latex, it has the water-soluble of excellence.Therefore be subjected to people's attention.The polyacrylamide series product can be divided into non-ionic type (NPAM), cationic (APAM) and anionic (CPAM) three major types.These polymkeric substance can be homopolymer, also can be multipolymers.The size of molecular weight is one of topmost performance index of polyacrylamide.
It is several that the production method of polyacrylamide mainly contains water solution polymerization process, suspension polymerization and inverse emulsion polymerization etc.Water solution polymerization process is the traditional method of producing polyacrylamide.Adopt this method can produce colloid and powder-like product.General polyacrylamide colloid is to adopt 8%～10% acrylamide solution direct polymerization and getting under the initiator effect.This colloid product is difficult for transportation, uses also inconvenient.But the production unit less investment, suitable small-sized manufacturing enterprise adopts.Polyacrylamide dry powder then more adopts 25%～30% acrylamide soln to carry out polymerization.The polyacrylamide colloid that obtains after the polymerization makes product after granulation, kneading, drying, pulverizing.Polyreaction wherein is a critical process.Advantage such as this method has production safety, processing unit is simple and production cost is low.Be to produce the method that polyacrylamide generally adopts both at home and abroad.But the particle of this series products formation is irregular, has shortcomings such as dissolving is slow, use is not thorough, postorder use equipment has high input.Reversed emulsion polymerization is with acrylamide and modified monomer (often soluble in water) thereof, is scattered in the non-polar liquid by water-in-oil type emulsifier, forms (W O) type emulsion and the polymerization carried out.Its molecular weight size, degree of hydrolysis, electric density and distribution thereof etc. have significant effects to its performance.Therefore synthetic relative molecular mass height, the uniform superpolymer of charge distribution become the target that people pursue.The stability of inverse emulsion polymerization product should keep some months at least in addition.From the latex products that will expect high solids content, high molecular weight, good stability that studies show that in the past, the profit proportioning in the building-up process, the selection of emulsifying agent initiator system and the use of amount etc. is the key factor that influences the latex products quality.
Summary of the invention
The objective of the invention is: at modified polyacrylamide colloid and power-product be difficult for dissolving, transportation use inconvenient, the production utilization ratio is low and in the market latex products exist relative molecular mass low, store technical deficiencies such as instability and carry out the optimization of technology and improve, a kind of new synthetic process of introducing different oxygen oximido group in the polyacrylamide macromole has been proposed.It has relative molecular mass height (weight average molecular mass can reach 2,000 ten thousand), and electric density is big, and latex is stablized (can reach 18 months storage period and layering floating oil caking phenomenon not occur), dissolution rate characteristics such as fast (dissolution time≤3 minute).
Technical scheme of the present invention: (be purchased certainly: be external phase Tianjin Red Hill general petrochemical works), acrylamide and modified monomer oxammonium hydrochloride thereof, the potassium acrylate aqueous solution are disperse phase with petroleum hydrocarbon 7# white oil.Selecting alkylphenol allyl polyether ethers response type surfactant active (be purchased certainly: the Guangzhou crowd is preced with U.S. trade Co., Ltds) and sorbitan sesquialter monoleate for use is emulsifying agent, and the mass ratio of two kinds of raw materials is 3～5: 1.
Profit under high shear, is made metastable latex, adopt azo diisobutyl amidine hydrochloric acid to make initiator, control initiated polymerization temperature is finished 30～90 ℃ of scopes.Its basic technology comprises the steps:
1) ratio in 1: 1～1.05 (w/w) is dissolved in acrylamide monomer in the resins exchange deionized water, and carries out corresponding activation treatment.
2) modified monomer oxammonium hydrochloride, potassium acrylate are carried out activation treatment.
3) with oil soluble promoting agent sorbitan sesquialter monoleate (be purchased from: be dissolved in oil phase Dandong oil chemistry factory), and in the corresponding high-shear emulsifying device of suction.
4) water-soluble active agent and water thorough mixing in container is even, and progressively add and carry out emulsification in the emulsor.
5) after emulsification is finished, emulsifying base is changed over to other reactor intensification and adds initiator 30～90 ℃ of scope intensification polymerizations.About 3～the 8h of polymerization time.
6) latex that polymerization is finished is warming up to 50～90 ℃, takes out the iso-hydroxamic modified polyacrylamide latex finished product that dense 2～5h promptly gets content about 50% in negative pressure 0.08Mpa～0.094Mpa scope vacuum.
Wherein: acrylamide ingredient requirement broad, no matter the acrylamide monomer of biological process or copper catalysis method all is applicable to this technology, and can both synthesize the latex products of relative molecular mass 〉=2,000 ten thousand.
Wherein: the range of choice broad to modified monomer both can also can be used cationic monomer with anionic property, and its modification degree also can be finished in the scope of broad simultaneously.This process using oxammonium hydrochloride and potassium acrylate are modified monomer.
Wherein: adopt and account for the ethers tensio-active agent alkylphenol allyl polyether ethers response type surfactant active of monomer content 6%～10% as comonomer.Oil soluble promoting agent and water-soluble active agent ratio are 3～5: 1
Wherein: oil-water ratio 1: 2.5～3.5 (w/w).
Wherein: initiator adopts the dual initiator segmentation to cause and finishes, and its azo diisobutyl amidine hydrochloric acid is 0.5～0.8: 1 with the mol ratio of hydrogen peroxide.
Advantage of the present invention is: compared with prior art technology requires low to the reactive behavior of polymerization single polymerization monomer.The acrylamide monomer that no matter is biochemical process and the production of copper catalysis method all can satisfy the production requirement of this technology, and can synthesize relative molecular mass greater than 2,000 ten thousand polymer latex; The emulsifying agent that adopts is participated in the polyreaction of function monomer directly.Introduce the stability that different oxygen oximido group improved latex (can guarantee finished product latex 18 months in no layering floating oil phenomenon); Use by compound emulsifying agent has simultaneously improved the dissolution dispersity of latex products can (generally in water dissolution time no longer than 3 minutes); This process using azo diisobutyl amidine hydrochloric acid and the segmentation of superoxide dual initiator cause, and make the polyreaction heat release be more prone to control, can breakdown of emulsion is not gluing, the narrowly distributing of polymericular weight because heat radiation is insufficient.
The iso-hydroxamic modified polyacrylamide latex products of explained hereafter of the present invention has 1. dissolution time weak point, and latex products is added in the entry, can dissolve rapidly to be scattered in exhausted gel-free body and insoluble micelle in the water within 3 minutes; General commercially available dry powder and colloid product dissolution time be about 1～3 hour, and gelinite and insoluble micelle inevitably can occur.2. molecular weight height, latex products are pressed GB/T12005.10-1992 and are detected, and molecular weight can reach more than 2,000 ten thousand.Be specially adapted to from bauxite, refine the red-mud settlement flocculation in the alumina technology process.
Below be that iso-hydroxamic modified polyacrylamide and commercially available polyacrylamide power-product compare in the application in this field:
Embodiment
For a better understanding of the present invention, according to technology solution of the present invention, further illustrate content of the present invention below, but content of the present invention not only is confined to following example in conjunction with example.
Embodiment 1: it be external phase with the aqueous solution of acrylamide, potassium acrylate and oxammonium hydrochloride is disperse phase that the present invention adopts the 7# white oil, under stirring, brute force forms stable emulsion, segmentation adds initiator azo diisobutyl amidine hydrochloric acid and the hydrogen peroxide initiated polymerization forms the modified polyacrylamide emulsion, through the high temperature negative pressure take out after dense finished product.Basic technology may further comprise the steps:
Pressed the profit volume ratio 1: 2.5, oxammonium hydrochloride: the acrylamide mol ratio is sampling in 1: 1.2 and adds emulsor emulsification, fill nitrogen then and be warming up to 30 ℃, 1: 10000～1: the 1000 azo diisobutyl amidine hydrochloric acid that adds amount of monomer, be warming up to 50 ℃ of hydrogen peroxide that add azo dibutyl amidine hydrochloric acid with molar weight again, initiated polymerization 6h.Reaction is warming up to 90 ℃ after finishing, and negative pressure is taken out the dense modified polyacrylamide latex that gets content 50%, molecular weight 〉=2,000 ten thousand.
Embodiment 2: it is external phase that the present invention adopts the 7# white oil, the aqueous solution with acrylamide, acrylate and oxammonium hydrochloride is disperse phase, under stirring, brute force forms stable emulsion, segmentation adds initiator azo diisobutyl amidine hydrochloric acid and the hydrogen peroxide initiated polymerization forms the modified polyacrylamide emulsion, through the high temperature negative pressure take out after dense finished product.Basic technology may further comprise the steps:
Pressed the profit volume ratio 1: 3, oxammonium hydrochloride: the acrylamide mol ratio is sampling in 1: 1.2 and adds emulsor emulsification, fill nitrogen then and be warming up to 30 ℃, 1: 10000～1: the 1000 azo diisobutyl amidine hydrochloric acid that adds amount of monomer, be warming up to 50 ℃ of hydrogen peroxide that add azo dibutyl amidine hydrochloric acid with molar weight again, initiated polymerization 6h.Reaction is warming up to 90 ℃ after finishing, and negative pressure is taken out the dense modified polyacrylamide latex that gets content 50%, molecular weight 〉=2,000 ten thousand.
Embodiment 3: it is external phase that the present invention adopts the 7# white oil, the aqueous solution with acrylamide, acrylate and oxammonium hydrochloride is disperse phase, under stirring, brute force forms stable emulsion, segmentation adds initiator azo diisobutyl amidine hydrochloric acid and the hydrogen peroxide initiated polymerization forms the modified polyacrylamide emulsion, through the high temperature negative pressure take out after dense finished product.Basic technology may further comprise the steps:
Pressed the profit volume ratio 1: 3.5, oxammonium hydrochloride: the acrylamide mol ratio is sampling in 1: 1.2 and adds emulsor emulsification, fill nitrogen then and be warming up to 30 ℃, 1: 10000～1: the 1000 azo diisobutyl amidine hydrochloric acid that adds amount of monomer, be warming up to 50 ℃ of hydrogen peroxide that add azo dibutyl amidine hydrochloric acid with molar weight again, initiated polymerization 6h.Reaction is warming up to 90 ℃ after finishing, and negative pressure is taken out the dense modified polyacrylamide latex that gets content 50%, molecular weight 〉=2,000 ten thousand.
Embodiment 4: it is external phase that the present invention adopts the 7# white oil, the aqueous solution with acrylamide, acrylate and oxammonium hydrochloride is disperse phase, under stirring, brute force forms stable emulsion, segmentation adds initiator azo diisobutyl amidine hydrochloric acid and the hydrogen peroxide initiated polymerization forms the modified polyacrylamide emulsion, through the high temperature negative pressure take out after dense finished product.Basic technology may further comprise the steps:
Pressed the profit volume ratio 1: 3, oxammonium hydrochloride: the acrylamide mol ratio is sampling in 1: 1.1 and adds emulsor emulsification, fill nitrogen then and be warming up to 30 ℃, 1: 10000～1: the 1000 azo diisobutyl amidine hydrochloric acid that adds amount of monomer, be warming up to 50 ℃ of hydrogen peroxide that add azo dibutyl amidine hydrochloric acid with molar weight again, initiated polymerization 6h.Reaction is warming up to 90 ℃ after finishing, and negative pressure is taken out the dense modified polyacrylamide latex that gets content 50%, molecular weight 〉=2,000 ten thousand
Embodiment 5: it is external phase that the present invention adopts the 7# white oil, the aqueous solution with acrylamide, acrylate and oxammonium hydrochloride is disperse phase, under stirring, brute force forms stable emulsion, segmentation adds initiator azo diisobutyl amidine hydrochloric acid and the hydrogen peroxide initiated polymerization forms the modified polyacrylamide emulsion, through the high temperature negative pressure take out after dense finished product.Basic technology may further comprise the steps:
Pressed the profit volume ratio 1: 3, oxammonium hydrochloride: the acrylamide mol ratio is sampling in 1: 1.2 and adds emulsor emulsification, fill nitrogen then and be warming up to 30 ℃, 1: 10000～1: the 1000 azo diisobutyl amidine hydrochloric acid that adds amount of monomer, be warming up to 50 ℃ of hydrogen peroxide that add azo dibutyl amidine hydrochloric acid with molar weight again, initiated polymerization 6h.Reaction is warming up to 90 ℃ after finishing, and negative pressure is taken out the dense modified polyacrylamide latex that gets content 50%, molecular weight 〉=2,000 ten thousand
Embodiment 6: it is external phase that the present invention adopts the 7# white oil, the aqueous solution with acrylamide, acrylate and oxammonium hydrochloride is disperse phase, under stirring, brute force forms stable emulsion, segmentation adds initiator azo diisobutyl amidine hydrochloric acid and the hydrogen peroxide initiated polymerization forms the modified polyacrylamide emulsion, through the high temperature negative pressure take out after dense finished product.Basic technology may further comprise the steps:
Pressed the profit volume ratio 1: 3, oxammonium hydrochloride: the acrylamide mol ratio is sampling in 1: 1.3 and adds emulsor emulsification, fill nitrogen then and be warming up to 30 ℃, 1: 10000～1: the 1000 azo diisobutyl amidine hydrochloric acid that adds amount of monomer, be warming up to 50 ℃ of hydrogen peroxide that add azo dibutyl amidine hydrochloric acid with molar weight again, initiated polymerization 6h.Reaction is warming up to 90 ℃ after finishing, and negative pressure is taken out the dense modified polyacrylamide latex that gets content 50%, molecular weight 〉=2,000 ten thousand.
Embodiment 7: it is external phase that the present invention adopts the 7# white oil, the aqueous solution with acrylamide, acrylate and oxammonium hydrochloride is disperse phase, under stirring, brute force forms stable emulsion, segmentation adds initiator azo diisobutyl amidine hydrochloric acid and the hydrogen peroxide initiated polymerization forms the modified polyacrylamide emulsion, through the high temperature negative pressure take out after dense finished product.Basic technology may further comprise the steps:
Pressed the profit volume ratio 1: 3, oxammonium hydrochloride: acrylamide (biochemical process production) mol ratio is sampling in 1: 1.2 and adds emulsor emulsification, fill nitrogen then and be warming up to 30 ℃, 1: 10000～1: the 1000 azo diisobutyl amidine hydrochloric acid that adds amount of monomer, be warming up to 50 ℃ of hydrogen peroxide that add azo dibutyl amidine hydrochloric acid with molar weight again, initiated polymerization 6h.Reaction is warming up to 90 ℃ after finishing, and negative pressure is taken out the dense modified polyacrylamide latex that gets content 50%, molecular weight 〉=2,000 ten thousand.
Embodiment 8: it is external phase that the present invention adopts the 7# white oil, the aqueous solution with acrylamide, acrylate and oxammonium hydrochloride is disperse phase, under stirring, brute force forms stable emulsion, segmentation adds initiator azo diisobutyl amidine hydrochloric acid and the hydrogen peroxide initiated polymerization forms the modified polyacrylamide emulsion, through the high temperature negative pressure take out after dense finished product.Basic technology may further comprise the steps:
Pressed the profit volume ratio 1: 3, oxammonium hydrochloride: the acrylamide mol ratio is sampling in 1: 1.2 and adds emulsor emulsification, fill nitrogen then and be warming up to 30 ℃, 1: 10000～1: the 1000 azo diisobutyl amidine hydrochloric acid that adds amount of monomer, be warming up to 50 ℃ of hydrogen peroxide that add azo dibutyl amidine hydrochloric acid with molar weight again, initiated polymerization 6h.Reaction is warming up to 90 ℃ after finishing, and negative pressure is taken out the dense modified polyacrylamide latex that gets content 50%, molecular weight 〉=2,000 ten thousand.
Claims (7)
1. the preparation method of an iso-hydroxamic modified polyacrylamide, it is characterized in that: with petroleum hydrocarbon 7# white oil is external phase, with acrylamide, oxammonium hydrochloride and potassium acrylate salt brine solution is disperse phase, add sorbitan sesquialter monoleate mutually respectively and alkylphenol allyl polyether ethers response type surfactant active is made metastable latex under high shear at profit, adopt azo diisobutyl amidine hydrochloric acid and the segmentation of hydrogen peroxide initiator to cause, the control kick off temperature is finished the about 3～8h of polymerization time 30～90 ℃ of scopes.
2. the preparation method of a kind of iso-hydroxamic modified polyacrylamide according to claim 1 is characterized in that: adopt oxammonium hydrochloride that polyacrylamide is carried out modification, acrylamide and oxammonium hydrochloride mol ratio are 1.1～1.3: 1.
3. the preparation method of a kind of iso-hydroxamic modified polyacrylamide according to claim 1 is characterized in that: adopting petroleum hydrocarbon 7# white oil is external phase, and water oil ratio is 1: 2.5～3.5.
4. the preparation method of a kind of iso-hydroxamic modified polyacrylamide according to claim 1, it is characterized in that: adopting sorbitan sesquialter monoleate and alkylphenol allyl polyether ethers response type surfactant active is emulsifying agent, and its mass ratio is: 3～5: 1.
5. the preparation method of a kind of iso-hydroxamic modified polyacrylamide according to claim 1, it is characterized in that: adopt azo diisobutyl amidine hydrochloric acid and hydrogen peroxide initiator to carry out the segmentation initiated polymerization, its initiator amount accounts for 1: 10000～1: 1000 of monomer consumption, and the mol ratio of azo diisobutyl amidine hydrochloric acid and hydrogen peroxide is 0.5～0.8: 1.
6. the preparation method of a kind of iso-hydroxamic modified polyacrylamide according to claim 1, it is characterized in that: the latex that polymerization is finished is warming up to 50～90 ℃, changes polyacrylamide latex finished product what negative pressure 0.08Mpa～0.094Mpa scope vacuum took out that dense 2～5h promptly gets content about 50%.
7. the preparation method of a kind of iso-hydroxamic modified polyacrylamide according to claim 1 is characterized in that: adopt and account for the ethers tensio-active agent alkylphenol allyl polyether ethers response type surfactant active of monomer content 6%～10% as comonomer.Oil soluble promoting agent and water-soluble active agent ratio are 3～5: 1.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103242489A (en) * | 2013-05-20 | 2013-08-14 | 安徽天润化学工业股份有限公司 | Preparation method of settling separation agent for red mud in aluminium ores |
| CN103524757A (en) * | 2012-07-04 | 2014-01-22 | 中国中化股份有限公司 | Preparation method of hydroxamic acid modified polyacrylamide emulsion flocculant |
| CN107043439A (en) * | 2017-03-30 | 2017-08-15 | 山东诺尔生物科技有限公司 | A kind of preparation method of aluminium ore dedicated separation agent |
| CN110804110A (en) * | 2019-10-31 | 2020-02-18 | 广东省石油与精细化工研究院 | High molecular weight hydroxamated polyacrylamide emulsion and preparation method thereof |
| CN112007762A (en) * | 2019-12-16 | 2020-12-01 | 中蓝连海设计研究院有限公司 | Positive flotation regulator for collophanite containing high sesquioxide, method and application |
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2009
- 2009-07-13 CN CN2009100631510A patent/CN101591415B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103524757A (en) * | 2012-07-04 | 2014-01-22 | 中国中化股份有限公司 | Preparation method of hydroxamic acid modified polyacrylamide emulsion flocculant |
| CN103524757B (en) * | 2012-07-04 | 2016-03-30 | 中国中化股份有限公司 | A kind of preparation method of hydroxamic acid modified polyacrylamide emulsion flocculant |
| CN103242489A (en) * | 2013-05-20 | 2013-08-14 | 安徽天润化学工业股份有限公司 | Preparation method of settling separation agent for red mud in aluminium ores |
| CN107043439A (en) * | 2017-03-30 | 2017-08-15 | 山东诺尔生物科技有限公司 | A kind of preparation method of aluminium ore dedicated separation agent |
| CN110804110A (en) * | 2019-10-31 | 2020-02-18 | 广东省石油与精细化工研究院 | High molecular weight hydroxamated polyacrylamide emulsion and preparation method thereof |
| CN110804110B (en) * | 2019-10-31 | 2022-05-24 | 广东省石油与精细化工研究院 | High molecular weight hydroxamated polyacrylamide emulsion and preparation method thereof |
| CN112007762A (en) * | 2019-12-16 | 2020-12-01 | 中蓝连海设计研究院有限公司 | Positive flotation regulator for collophanite containing high sesquioxide, method and application |
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