CN110804110A - High molecular weight hydroxamated polyacrylamide emulsion and preparation method thereof - Google Patents

High molecular weight hydroxamated polyacrylamide emulsion and preparation method thereof Download PDF

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CN110804110A
CN110804110A CN201911049424.6A CN201911049424A CN110804110A CN 110804110 A CN110804110 A CN 110804110A CN 201911049424 A CN201911049424 A CN 201911049424A CN 110804110 A CN110804110 A CN 110804110A
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oil phase
phase
oil
emulsion
polyacrylamide emulsion
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CN110804110B (en
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缪飞
栾安博
邱美坚
冯璐
汤小燕
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Guangdong Petroleum And Fine Chemical Research Institute
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F8/00Chemical modification by after-treatment
    • C08F8/30Introducing nitrogen atoms or nitrogen-containing groups
    • C08F8/32Introducing nitrogen atoms or nitrogen-containing groups by reaction with amines
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/12Polymerisation in non-solvents
    • C08F2/16Aqueous medium
    • C08F2/22Emulsion polymerisation
    • C08F2/24Emulsion polymerisation with the aid of emulsifying agents
    • C08F2/30Emulsion polymerisation with the aid of emulsifying agents non-ionic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/52Amides or imides
    • C08F220/54Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
    • C08F220/58Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine

Abstract

The invention provides a high molecular weight hydroxamated polyacrylamide emulsion and a preparation method thereof, wherein the preparation method comprises the following steps: s1: mixing a monomer and sodium hypophosphite, and adjusting the pH value with liquid alkali to obtain a water phase; adding sorbitan fatty acid ester and coconut oil fatty acid diethanolamide into the oil phase matrix to form an oil phase; mixing the water phase and the oil phase, and carrying out polymerization reaction under the action of ammonium persulfate and at 45-50 ℃ in an inert atmosphere to obtain a polyacrylamide emulsion; s2: adding sodium thiosulfate and liquid caustic soda into a hydroxylamine sulfate aqueous solution to prepare a water phase; mixing industrial ethoxylated fatty amine with industrial solvent oil to form an oil phase; dispersing the polyacrylamide emulsion in an oil phase, adding a water phase, and reacting at 25-45 ℃ for more than 1.5h to obtain the polyacrylamide emulsion. The invention can obtain high-stability high-molecular-weight hydroxamated polyacrylamide emulsion at lower temperature by reasonably selecting raw materials and processes, and reduces the loss of molecular weight before and after hydroxamation.

Description

High molecular weight hydroxamated polyacrylamide emulsion and preparation method thereof
Technical Field
The invention belongs to the technical field of polymer synthesis, and particularly relates to a high molecular weight hydroxamated polyacrylamide emulsion and a preparation method thereof.
Background
The hydroxamated polyacrylamide emulsion is a common flocculant for separating red mud in the process of producing alumina by a Bayer process, and compared with a conventional flocculant, the hydroxamated polyacrylamide emulsion has the advantages of small addition amount, high settling velocity, low content of overflow suspended matters, high solid content of underflow and the like, and small flocculus formed in the using process is firmer. In the flocculation process of the hydroxamated polyacrylamide emulsion on the red mud, the hydroxamate functional group in the hydroxamated polyacrylamide emulsion is utilized to chelate metal elements in the red mud, so that the hydroxamate functional group is adsorbed on the surface of red mud particles to be settled. The size of the molecular weight of the hydroxamated polyacrylamide has great influence on the flocculation capacity of the red mud, and generally, the larger the molecular weight is, the larger the adsorption capacity is, and the better the flocculation effect is.
In the prior art scheme, two processes are mainly used for preparing the hydroxamated polyacrylamide emulsion. One is that hydroxylamine salt is used as functional monomer to directly participate in emulsion polymerization reaction. For example, CN101591415A uses unneutralized hydroxylamine hydrochloride as a modifying monomer to participate in the emulsion polymerization reaction under acidic conditions that limit the reaction rate, but the extreme temperatures (e.g., 90 ℃) used can cause emulsion instability. In the preparation method of the hydroxamic acid type polyacrylamide inverse emulsion of CN109180862A, an aqueous solution of a hydroxamic acid monomer is prepared at first, then the hydroxamic acid monomer is stirred with acrylamide and acrylic acid to be dissolved, and then ammonia water is used for adjusting the pH value to 7-9 to prepare a water phase; then preparing W/O pre-emulsion, adding initiator to initiate polymerization reaction, and finally adding phase reversal agent. Similar to CN101591415A, the reaction temperature of the scheme is higher (up to 80 ℃), and the stability of the product is seriously influenced.
The other method is to synthesize the polyacrylamide microemulsion or emulsion first and then carry out hydroxamic acid modification. For example, CN104528905A uses an aqueous solution of ammonium acrylate and acrylamide as a comonomer, and cyclohexane as a continuous phase, and performs inverse microemulsion polymerization, and then performs hydroxamic acid modification with hydroxylamine hydrochloride. The emulsion polymerization temperature of the scheme is high, and the hydroxamic acidification reaction is high in temperature and long in time, and is easy to cause the degradation of the molecular weight of the polymer (without a stabilizer). CN103524757A takes acrylamide and acrylic acid as polymerization monomers, a water-in-oil emulsion with the viscosity average molecular weight of about 1500 ten thousand is obtained by an emulsion polymerization method, then hydroxamic acid modification is carried out, and phase inversion is carried out to obtain the oil-in-water hydroxamic acid modified polyacrylamide emulsion flocculant, but the problems of overhigh temperature (80 ℃) and long time of the later hydroxamic acid modification reaction still exist.
In summary, the prior art generally performs a polyacrylamide emulsion polymerization reaction and hydroxamic acid modification at a high temperature, and due to the fact that the brownian motion of emulsion colloidal particles is aggravated due to the excessively high reaction temperature, the rate of coalescence caused by collision among the emulsion colloidal particles is increased, and the stability of the emulsion is reduced; furthermore, the temperature increase causes the reduction of the hydrated layer on the surface of the latex particles, which also leads to a decrease in the stability of the emulsion. Meanwhile, the hydroxamation reaction at a relatively high temperature promotes the reaction between the polymer and hydroxylamine, but the decomposition of hydroxylamine (the amount of hydroxylamine used is excessively large) and the reaction is difficult due to the increase in the viscosity of the system, which requires a long reaction time.
Disclosure of Invention
The invention aims to solve the problem of overhigh reaction temperature in the existing production process of the hydroxamated polyacrylamide emulsion, and provides a high molecular weight hydroxamated polyacrylamide emulsion and a preparation method thereof.
The high molecular weight hydroxamated polyacrylamide emulsion provided by the invention has a molecular weight of more than or equal to 1700 ten thousand and a solid content of more than or equal to 20%.
Further, the viscosity of the high molecular weight hydroxamated polyacrylamide emulsion at 27 ℃ is 4200-4900 cP.
The preparation method of the high molecular weight hydroxamated polyacrylamide emulsion provided by the invention comprises the following steps:
s1: emulsion polymerization process
(1) Preparation of the aqueous phase: adding acrylic acid into a 2-acrylamide-2-methylpropanesulfonic acid aqueous solution, adjusting the pH value to 7.5-8 by using liquid alkali at the temperature of not higher than 20 ℃, and then adding acrylamide and sodium hypophosphite to perform a prepolymerization reaction to obtain a comonomer water phase;
(2) preparation of oil phase: adding sorbitan fatty acid ester and coconut oil fatty acid diethanolamide into the oil phase matrix to form an oil phase, wherein the total amount of the sorbitan fatty acid ester and the coconut oil fatty acid diethanolamide accounts for 11-12% (wt) of the oil phase;
(3) emulsion polymerization: mixing a comonomer water phase and an oil phase according to the mass ratio of (3-4) to (1) to form a water-in-oil type emulsion, and then carrying out polymerization reaction under the action of ammonium persulfate and at 45-50 ℃ in an inert atmosphere to obtain a polyacrylamide emulsion;
s2: oxime acidification process
(1) Preparation of the aqueous phase: adding sodium thiosulfate and liquid caustic soda into a hydroxylamine sulfate aqueous solution to prepare a water phase;
(2) preparation of oil phase: mixing industrial ethoxylated fatty amine with industrial solvent oil to form an oil phase;
(3) hydroxamation reaction: dispersing the polyacrylamide emulsion in an oil phase, adding a water phase, and reacting at 25-45 ℃ for more than 1.5h to obtain the water-in-oil type high-molecular-weight hydroxamic acid polyacrylamide emulsion.
Further, the molecular weight of the polymer in the polyacrylamide emulsion in step S1 is not less than 1800 ten thousand.
Furthermore, the molar ratio of the 2-acrylamide-2-methylpropanesulfonic acid to the acrylic acid to the acrylamide to the sodium hypophosphite in the step (1) is (55-60): (25-30): (15-20): 0.11-0.2).
Further, in step S1, the oil phase matrix in the oil phase is liquid paraffin.
Furthermore, the mass ratio of the sorbitan fatty acid ester to the coconut oil fatty acid diethanolamide in the oil phase in the step S1 is (8-9): 1.
Further, the mass ratio of the industrial solvent oil to the industrial ethoxylated fatty amine in the oil phase in the step S2 is (12-15): 1.
The industrial ethoxylated fatty amine EO is 2-8 and contains a C10-C20 fatty alkyl group.
Further, in the step S2, the mass ratio of the water phase to the oil phase to the polyacrylamide emulsion is 18 (6-15): (30-36).
Compared with the prior art, the invention adopts 11-12 percent (wt) of sorbitan fatty acid ester and coconut oil fatty acid diethanolamide composite emulsifier to regulate the oil phase in the emulsion polymerization process, and adopts industrial solvent oil as the oil phase matrix in the hydroxamic acidification process, thereby effectively avoiding reaction difficulty caused by overlarge viscosity after the hydrolysis of the polymer, improving the hydroxylamine conversion rate in the hydroxamic acidification process and shortening the reaction time. Meanwhile, the hydroxamic acid reaction is carried out at the low temperature of 25-45 ℃, so that the proper viscosity and stability of a maintenance system are facilitated, and the volatilization of industrial solvent oil can be prevented.
In addition, in the process of hydroxamic acidification, liquid alkali (sodium hydroxide or potassium hydroxide) and hydroxylamine sulfate are used for generating hydroxylamine in an aqueous solution, the hydroxylamine and a polymer undergo nucleophilic substitution reaction under the catalysis condition of high-concentration alkali, and meanwhile, the hydroxylamine stabilizer sodium thiosulfate can be used for effectively preventing the hydroxylamine from degrading and reducing the loss of the molecular weight of the polymer.
Drawings
FIG. 1 is an optical micrograph of a polyacrylamide emulsion according to example 1;
FIG. 2 is an optical micrograph of a hydroxamated polyacrylamide emulsion according to example 1.
Detailed Description
The technical solution of the present invention will be described below with reference to specific examples.
Example 1
The preparation method of the high molecular weight hydroxamated polyacrylamide emulsion provided in this example is as follows:
s1: emulsion polymerization process
(1) Preparation of the aqueous phase: dissolving a monomer 2-acrylamide-2-methylpropanesulfonic Acid (AMPS) in deionized water under stirring to prepare a 50% (wt) aqueous solution, then adding a monomer Acrylic Acid (AA), and adjusting the pH to be approximately equal to 8 by using 42% (wt) liquid alkali (the control temperature is not higher than 20 ℃); then adding monomer Acrylamide (AM) and deionized water to prepare aqueous solution with monomer concentration of 50 percent (wt). Adding initiator Sodium Hypophosphite (SHP) into the aqueous solution to initiate prepolymerization reaction to form a comonomer aqueous phase. Wherein the molar ratio of AM, AA, AMPS and SHP is 60:25:15: 0.11.
(2) Preparation of oil phase: adding a composite emulsifier of Span-80 (sorbitan fatty acid ester) and 6501 (coconut fatty acid diethanolamide) into liquid paraffin under stirring to prepare an oil phase, wherein the mass ratio of Span-80 to 6501 is 9: 1; the total amount of emulsifier was 11.5% (wt) of the oil phase.
(3) Emulsion polymerization: adding the water phase and the oil phase (the mass ratio of the water phase to the oil phase is 3.75:1) into a hinged blade paddle stirrer with an enamel inner wall, mixing, and carrying out high-speed shearing stirring for about 15min to form the water-in-oil emulsion. Then the stirring speed is controlled at about 300rpm, and after nitrogen is introduced for 30min to fully remove oxygen, the initiator Ammonium Persulfate (APS) with the dosage of 0.21% (mol) of the monomer is added to initiate the polymerization reaction. The temperature rise is controlled at 1 ℃/5min in the polymerization reaction process, the temperature is controlled by ice water after the temperature rises to 45 ℃, and the final temperature is controlled not to exceed 50 ℃. And after continuing to react for 4 hours, stopping introducing nitrogen to finish the reaction to obtain the polyacrylamide emulsion.
S2: oxime acidification process
(1) Preparation of the aqueous phase: 10 parts by weight of hydroxylamine stabilizer sodium thiosulfate was added to 138 parts of 30% (wt) hydroxylamine sulfate aqueous solution under stirring, after complete dissolution, 132 parts of 42% (wt) liquid alkali was slowly added, and the temperature was maintained below 20 ℃ with an ice water bath as an aqueous phase. The aqueous phase was left at room temperature for 4 h.
(2) Preparation of oil phase: the 100# mineral spirits were mixed with 1805 (commercial ethoxylated fatty amine, EO ═ 5 (i.e. 5 ethoxy number), C10-C20 fatty alkyl group) at a mass ratio of 12:1, and stirred to give a clear oil phase.
(3) Hydroxamation reaction: adding 30 parts by weight of the polyacrylamide emulsion prepared in the step S1 into a stainless steel interlayer charging barrel, adding 7 parts by weight of an oil phase, and dispersing for 10min to thin a mixed system; then adding 18 parts of water phase, carrying out hydroxamic acidification reaction under high-speed stirring, and gradually thickening the system in the reaction process. The total hydroxamic acidification reaction time is controlled to be more than 1.5h (preferably 2-2.5 h), and the reaction temperature is controlled to be 25-45 ℃. And obtaining the water-in-oil type high molecular weight hydroxamic acid polyacrylamide emulsion after the reaction is finished.
Example 2
The preparation method of the high molecular weight hydroxamated polyacrylamide emulsion provided in this example is as follows:
s1: emulsion polymerization process
The same as step S1 in example 1.
S2: oxime acidification process
(1) Preparation of the aqueous phase: the same as in step S2(1) of example 1.
(2) Preparation of oil phase: 120# solvent oil was mixed with 1802 (industrial ethoxylated fatty amine, EO ═ 2) in a mass ratio of 13.5:1, and stirred uniformly to obtain a clear oil phase.
(3) Hydroxamation reaction: adding 35 parts by weight of the polyacrylamide emulsion prepared in the step S1 into a stainless steel interlayer charging barrel, adding 7 parts by weight of an oil phase, dispersing for 10min, adding 18 parts by weight of a water phase, carrying out a hydroxamic acidification reaction at 25-45 ℃, and reacting for 2.5h to obtain the water-in-oil type high molecular weight hydroxamic polyacrylamide emulsion.
Example 3
The preparation method of the high molecular weight hydroxamated polyacrylamide emulsion provided in this example is as follows:
s1: emulsion polymerization process
The same as step S1 in example 1.
S2: oxime acidification process
(1) Preparation of the aqueous phase: the same as in step S2(1) of example 1.
(2) Preparation of oil phase: 150# solvent oil was mixed with 1802 (industrial ethoxylated fatty amine, EO ═ 2) in a mass ratio of 14:1, and stirred to give a clear oil phase.
(3) Hydroxamation reaction: adding 32 parts by weight of the polyacrylamide emulsion prepared in the step S1 into a stainless steel interlayer charging barrel, adding 9 parts by weight of an oil phase, dispersing for 10min, adding 18 parts by weight of a water phase, carrying out a hydroxamic acidification reaction at 25-45 ℃, and reacting for 2h to obtain the water-in-oil type high molecular weight hydroxamic polyacrylamide emulsion.
Example 4
The preparation method of the high molecular weight hydroxamated polyacrylamide emulsion provided in this example is as follows:
s1: emulsion polymerization process
The same as step S1 in example 1.
S2: oxime acidification process
(1) Preparation of the aqueous phase: the same as in step S2(1) of example 1.
(2) Preparation of oil phase: mixing 150# solvent oil with 1802 and 1805 composite emulsifier (mass ratio of 2:1) according to the mass ratio of 15:1, and stirring to obtain clear oil phase.
(3) Hydroxamation reaction: adding 36 parts by weight of the polyacrylamide emulsion prepared in the step S1 into a stainless steel interlayer charging barrel, adding 11 parts by weight of an oil phase, dispersing for 10min, adding 18 parts by weight of a water phase, carrying out a hydroxamic acidification reaction at 25-45 ℃, and reacting for 2.5h to obtain the water-in-oil type high molecular weight hydroxamic polyacrylamide emulsion.
Example 5
The preparation method of the high molecular weight hydroxamated polyacrylamide emulsion provided in this example is as follows:
s1: emulsion polymerization process
The detailed steps are the same as step S1 in embodiment 1.
S2: oxime acidification process
(1) Preparation of the aqueous phase: the same as in step S2(1) of example 1.
(2) Preparation of oil phase: mixing the 120# solvent oil with 1802 and 1805 composite emulsifier (mass ratio is 1:1) according to the mass ratio of 13:1, and stirring to obtain a clear oil phase.
(3) Hydroxamation reaction: adding 33 parts by weight of the polyacrylamide emulsion prepared in the step S1 into a stainless steel interlayer charging barrel, adding 10 parts by weight of an oil phase, dispersing for 10min, adding 18 parts by weight of a water phase, carrying out a hydroxamic acidification reaction at 25-45 ℃, and reacting for 2h to obtain the water-in-oil type high molecular weight hydroxamic polyacrylamide emulsion.
With reference to the method of GB/T17514-.
TABLE 1 Properties of the Polyacrylamide emulsions and hydroxamated Polyacrylamide emulsions of examples 1 to 5
Figure BDA0002254941990000061
Table 1 reflects that the relative molecular weight of the polyacrylamide emulsion polymer of step S1 was as high as 1827 ten thousand, and the polymer solids content was 38.74% (wt). As can be seen from the optical micrograph of the polyacrylamide emulsion shown in FIG. 1, the particle size distribution of the latex particles in the polyacrylamide emulsion is relatively wide, and the small latex particles are filled in the gaps between the large latex particles, so that the stacking density of the latex particles is increased, and the solid content of the polymer in the emulsion is increased.
The relative molecular mass of the polymer in the hydroxamated polyacrylamide in example 1 was 1768 ten thousand, and the loss was very small as compared with the relative molecular mass of the polymer before hydroxamation, and the solid content was 21.13%. As can be seen from the optical micrograph of the hydroxamated polyacrylamide emulsion in FIG. 2, the particle size of the latex particles in the hydroxamated polyacrylamide emulsion is less than 20 μm. And the hydroxamated polyacrylamide emulsion is uniform, fine and smooth, does not delaminate and has no visible gel block.
Similarly, the relative molecular mass of the polymer in the hydroxamated polyacrylamide emulsion of examples 2-5 changed very little from the relative molecular mass before hydroxamation, and the solid content of the polymer was between 20.97% (wt) and 22.60% (wt). The hydroxamated polyacrylamide emulsion is uniform, fine and smooth, does not delaminate, has no visible gel block, and has the viscosity of 4365.95-4879.94 cP at the temperature of 27 ℃.
Various factors such as the type and proportion of monomers, the type and concentration of emulsifiers, the type and concentration of initiators, phase ratios, stirring intensity, reaction temperature and other process parameters in the emulsion polymerization system and the emulsion polymerization process are mutually related organic integers, and have important influence on the quality of emulsion polymers. Compared with the prior art, the invention uses ammonium persulfate and sodium hypophosphite to form an oxidation-reduction initiation system in the polymerization process of the polyacrylamide emulsion, avoids using organic peroxide and azo compounds with higher toxicity which need to be stored at low temperature, reduces the cost and improves the storage and use safety; the polyacrylamide emulsion polymerization reaction is carried out at the low temperature of 45-50 ℃, so that the stability of the polyacrylamide emulsion can be effectively improved; by comprehensively balancing the process parameters such as the type, concentration, phase ratio, stirring strength and the like of the emulsifier and selecting the stirrer, the generation of gel in the polymerization process is reduced or avoided to the greatest extent; the particle size distribution of the latex particles in the polyacrylamide emulsion is wider, and the small latex particles are filled in gaps among large latex particles, so that the stacking density of the latex particles is increased, and the solid content and the molecular weight of the emulsion are improved. Meanwhile, the method carries out the hydroxamation reaction at 25-45 ℃, controls the hydroxamation reaction time to be more than 1.5h, can effectively reduce the loss of the molecular weight of the polymer in the hydroxamation reaction process without high temperature and long time, and can improve the production efficiency.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. A high molecular weight hydroxamated polyacrylamide emulsion is characterized in that: the relative molecular mass of the polymer in the high molecular weight hydroxamated polyacrylamide emulsion is more than or equal to 1700 ten thousand, and the solid content of the polymer is more than or equal to 20 percent.
2. The high molecular weight hydroxamated polyacrylamide emulsion according to claim 1, wherein: the viscosity of the high-molecular hydroxamated polyacrylamide emulsion at 27 ℃ is 4200-4900 cP.
3. A preparation method of high molecular weight hydroxamated polyacrylamide emulsion is characterized by comprising the following steps: the method comprises the following steps:
s1: emulsion polymerization process
(1) Preparation of the aqueous phase: adding acrylic acid into a 2-acrylamide-2-methylpropanesulfonic acid aqueous solution, adjusting the pH value to 7.5-8 by using liquid alkali at the temperature of not higher than 20 ℃, and then adding acrylamide and sodium hypophosphite to perform a prepolymerization reaction to obtain a comonomer water phase;
(2) preparation of oil phase: adding sorbitan fatty acid ester and coconut oil fatty acid diethanolamide into the oil phase matrix to form an oil phase, wherein the total amount of the sorbitan fatty acid ester and the coconut oil fatty acid diethanolamide accounts for 11-12% (wt) of the oil phase;
(3) emulsion polymerization: mixing a comonomer water phase and an oil phase according to the mass ratio of (3-4) to (1) to form a water-in-oil type emulsion, and then carrying out polymerization reaction under the action of ammonium persulfate and at 45-50 ℃ in an inert atmosphere to obtain a polyacrylamide emulsion;
s2: oxime acidification process
(1) Preparation of the aqueous phase: adding sodium thiosulfate and liquid caustic soda into a hydroxylamine sulfate aqueous solution to prepare a water phase;
(2) preparation of oil phase: mixing industrial ethoxylated fatty amine with industrial solvent oil to form an oil phase;
(3) hydroxamation reaction: dispersing the polyacrylamide emulsion in an oil phase, adding a water phase, and reacting at 25-45 ℃ for more than 1.5h to obtain the water-in-oil type high-molecular-weight hydroxamic acid polyacrylamide emulsion.
4. The method according to claim 3, wherein: and S1, the molecular weight of the polymer in the polyacrylamide emulsion is more than or equal to 1800 ten thousand.
5. The method according to claim 3, wherein: step S1, the molar ratio of 2-acrylamide-2-methyl propanesulfonic acid, acrylic acid, acrylamide and sodium hypophosphite in the aqueous phase is (55-60): (25-30): 15-20): 0.11-0.2.
6. The method according to claim 3, wherein: the oil phase matrix in the oil phase in the step S1 is liquid paraffin.
7. The method according to claim 3, wherein: the mass ratio of the sorbitan fatty acid ester to the coconut oil fatty acid diethanolamide in the oil phase in the step S1 is (8-9): 1.
8. The method according to claim 3, wherein: the mass ratio of the industrial solvent oil to the industrial ethoxylated fatty amine in the oil phase in the step S2 is (12-15): 1.
9. The method of claim 8, wherein: the industrial ethoxylated fatty amine EO is 2-8 and contains C10-C20 fatty alkyl.
10. The method according to claim 3, wherein: in the step S2, the mass ratio of the water phase to the oil phase to the polyacrylamide emulsion is 18 (6-15): (30-36).
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CN101658736A (en) * 2005-02-25 2010-03-03 Cytec技术有限公司 Water-in-oil-in water emulsions of hydroxamated polymers and methods for using the same
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
CN109180862A (en) * 2018-09-20 2019-01-11 江苏富淼科技股份有限公司 A kind of preparation method of hydroxamic acid polyacrylamide reversed-phase emulsion

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Publication number Priority date Publication date Assignee Title
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CN101658736A (en) * 2005-02-25 2010-03-03 Cytec技术有限公司 Water-in-oil-in water emulsions of hydroxamated polymers and methods for using the same
CN101591415A (en) * 2009-07-13 2009-12-02 湖北同一石油化工有限公司 Iso-hydroxamic modified polyacrylamide and preparation method thereof
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
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