CN107226875A - A kind of preparation method of reversed phase latex of polyacrylamide - Google Patents
A kind of preparation method of reversed phase latex of polyacrylamide Download PDFInfo
- Publication number
- CN107226875A CN107226875A CN201710547581.4A CN201710547581A CN107226875A CN 107226875 A CN107226875 A CN 107226875A CN 201710547581 A CN201710547581 A CN 201710547581A CN 107226875 A CN107226875 A CN 107226875A
- Authority
- CN
- China
- Prior art keywords
- polyacrylamide
- polymerization
- product
- reversed
- reversed phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers 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
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/52—Amides or imides
- C08F120/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F120/56—Acrylamide; Methacrylamide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/32—Polymerisation in water-in-oil emulsions
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers 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
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention belongs to water-soluble high-molecular material field, particularly a kind of method of industrially prepared reversed phase latex of polyacrylamide.The present invention obtains reversed phase latex of polyacrylamide product using multistep polymerization method.The first step is using acrylamide, acrylic acid or the methyl propane sulfonic acid of 2 acrylamido 2 as polymerized monomer, this disk class and OPEO (OP) are emulsifying agent, first a small amount of polymerization prepares reversed phase latex of polyacrylamide, heat of polymerization is few, it is ensured that will not occur in polymerization process because not in time the danger of implode occurs for radiating；Second step polymerization is further polymerize on the basis of first step polymerization, due to partially polymerized, and the heat of polymerization that second step polymerization is produced greatly reduces, and equally will not also occur also produce gel or demulsification in the phenomenon of implode, polymerization process.As long as follow-up polymerization process releases a part of product every time, the amount of releasing is determined according to the size and exothermal efficiency of polymeric kettle.This method can greatly improve the security of polymerisation, can use large-scale polymeric kettle and without worrying the possibility of implode, it is ensured that industrial steady safety is carried out.
Description
Technical field
The present invention relates to water-soluble high-molecular material field, particularly a kind of industrially prepared reversed phase latex of polyacrylamide
Method.
Background technology
With the development of polymerization technique, polyacrylamide develops into present dry powder by initial dry powder (colloid), anti-
Two kinds of major products of phase emulsion.Acrylamide powder product has dissolution time length and easily sheared by stirring in use
Degraded, need to be equipped with the drawbacks such as special dry powder dissolver.Reversed-phase emulsion is fast with dissolution velocity compared with dry powder, molecular weight
High and narrowly distributing, the few advantage of residual monomer, viscosity is small in polymerisation in addition, is suitable for large-scale production, and polyacrylamide is anti-
Phase emulsion progressively turns into the main flow of polyacrylamide amine product.But it is too high that the product has an emulsifier content, polymerize in addition
Journey is high due to monomer concentration, and polymerization heat is big, and common polymeric kettle is difficult that timely radiating causes implode or gel, or even is rushed
The accidents such as material.
The content of the invention
It can industrially stablize polymerization, emulsification it is an object of the invention to overcome the deficiencies of the prior art and provide one kind
The preparation method of the low reversed phase latex of polyacrylamide of agent content.
A kind of preparation method of reversed phase latex of polyacrylamide, it is characterized in that comprising the following steps：
(1) acrylamide aqueous solution that mass concentration is 30-50% is sequentially added in the batching kettle with agitator, added
Acrylamide monomer quality 0-5% anhydrous sodium acetate is accounted for, then acrylamide mole is accounted for by required anion degree addition
0-50% acrylic acid or 2- acrylamide-2-methylpro panesulfonic acids, the sodium hydrate aqueous solution for being 10-50% with mass concentration
The pH value of regulating system is 3-7, adds this certain proportion of disk class emulsifying agent and octyl phenol for accounting for monomer gross mass 8-30%
APEO (OP) series emulsifying agent, opens stirring, until reactant is well mixed；Then add and account for acrylamide aqueous solution
Volume 60-120% organic solvent；
(2) reversed-phase emulsion for obtaining step (1) in batching kettle is added to gentle equipped with agitator, thermometer, condenser
In the polymeric kettle that body is imported and exported, lead to nitrogen or carbon dioxide flooding oxygen, it is 5-35 DEG C to control temperature, stirs 30-60min, and chemistry draws
Hair or ultraviolet light initiated polymerization, reaction obtain reversed phase latex of polyacrylamide semi-finished product after terminating；
(3) this step is identical with step (1), and the total amount of dispensing releases reversed phase latex of polyacrylamide product for step (4)
Total amount；
(4) reversed-phase emulsion for preparing step (3) in batching kettle in whipping process is added slowly to poly- in step (2)
In acrylamide reversed-phase emulsion product, lead to nitrogen or carbon dioxide flooding oxygen, it is 5-35 DEG C to control temperature, stirs 30-60min, is changed
Learn and trigger or ultraviolet light initiated polymerization, reaction obtains reversed phase latex of polyacrylamide finished product after terminating；According to reaction
Kettle size and radiating efficiency, calculate or are drawn by experiment the optimised quantity for releasing product after reaction every time, release corresponding poly-
Acrylamide reversed-phase emulsion product, releases the reversed phase latex of polyacrylamide product for accounting for 0.3-0.7 times of total amount.
In principal character step (1) and step (3), during organic solvent is kerosene, atoleine, solvent naphtha or hexamethylene
It is a kind of；This disk class emulsifying agent is one kind in this disk 20, this disk 40, this disk 60, span 80 or this disk 85；Octyl phenol polyoxyethylene
Ether (OP) series emulsifying agent is one kind in OP-4, OP-6, OP-8, OP-10, OP-15, OP-20 or OP-30.
The present invention obtains reversed phase latex of polyacrylamide product using multistep polymerization method.The first step first a small amount of polymerization prepares poly-
Acrylamide reversed-phase emulsion, heat of polymerization is few, it is ensured that will not occur in polymerization process because not in time implode occurs for radiating
It is dangerous；Second step polymerization is further polymerize on the basis of first step polymerization, due to partially polymerized, second step polymerization production
Raw heat of polymerization greatly reduces, the phenomenon that equally will not also occur implode, and gel or demulsification will not be also produced in polymerization process.Afterwards
As long as continuous polymerization process releases a part of product every time, the amount of releasing is determined according to the size and exothermal efficiency of polymeric kettle.This
Kind of method can greatly improve the security of polymerisation, can use large-scale polymeric kettle and can without worry implode
Can, it is ensured that industrial steady safety is carried out.
The reversed phase latex of polyacrylamide that the present invention is obtained can be widely used in flocculating, thicken, drag reduction, gel, bonding, resistance
The fields such as dirt, particularly sewage disposal and oil exploitation industry.
Embodiment
Three most preferred embodiments of the present invention are given below：
Example one
The first step：43wt% acrylamide aqueous solution 1000kg is sequentially added in 3000 liters of batching kettle, is added
20kg anhydrous sodium acetates, add emolsifier span 60 (sorbitan monostearate) 75kg and OP-10 25kg, stirring
After 30min, hexamethylene 750kg is added,
Second step：It will be added to after the reversed-phase emulsion prepared of the first step in 5000 liters of polymeric kettles, adjust 15 DEG C of temperature, simultaneously
Logical carbon dioxide stirs 40min with the oxygen in removing system.The ammonium persulfate aqueous solution 0.5kg's and 5% for plus 1% afterwards
Aqueous solution of sodium bisulfite 1kg initiation reactions, rise to after maximum temperature, insulation reaction 1h, non-ionic polyacrylamide are made anti-
Phase emulsion semi-finished product.
3rd step：43wt% acrylamide aqueous solution 1000kg is sequentially added in the batching kettle vacated, 20kg is added
Anhydrous sodium acetate, adds after 75kg the and OP-10 25kg of emolsifier span 60, stirring 30min, adds hexamethylene 750kg.
4th step：The reversed-phase emulsion that the 3rd step is prepared is added slowly to second step polyacrylamide under agitation anti-
In phase emulsion, lead to carbon dioxide flooding oxygen, adjustment temperature stirs 40min to 25 DEG C, the ammonium persulfate aqueous solution 0.5kg for plus 1% and
5% aqueous solution of sodium bisulfite 1kg triggers, and rises to after maximum temperature, insulation reaction 1h, non-ionic polyacrylamide is made anti-
Phase emulsion finished product, the half that total amount is released afterwards is used as product.
Product can continuously be obtained by repeating the 3rd step and the 4th step.
Example two
The first step：41wt% acrylamide aqueous solution 750kg is sequentially added in 3000 liters of batching kettle, is added
The pH value for the sodium hydrate aqueous solution regulating system for being 30% with mass concentration under the conditions of 100kg acrylic acid, ice-water bath is 5.0.
Add after emolsifier span 80 (sorbitan mono-oleic acid ester) 75kg and OP-10 25kg, stirring 30min, add hexamethylene
750kg。
Second step：It will be added to after the reversed-phase emulsion prepared of the first step in 5000 liters of polymeric kettles, adjust 15 DEG C of temperature, simultaneously
Logical high pure nitrogen stirs 40min with the oxygen in removing system.The ammonium persulfate aqueous solution 0.5kg's and 5% for plus 1% afterwards
Aqueous solution of sodium bisulfite 0.5kg is risen to after maximum temperature with triggering, insulation reaction 1h, PAMA is made anti-
Phase emulsion semi-finished product.
3rd step：41wt% acrylamide aqueous solution 750kg is sequentially added in the batching kettle vacated, 100kg is added
The pH value for the sodium hydrate aqueous solution regulating system for being 30% with mass concentration under the conditions of acrylic acid, ice-water bath is 5.0, adds breast
After agent span 80 75kg and OP-10 25kg, stirring 30min, hexamethylene 750kg is added.
4th step：It is anti-phase that the reversed-phase emulsion that the 3rd step is prepared under agitation is added slowly to second step polyacrylamide
In emulsion, lead to High Purity Nitrogen gas drive oxygen, adjustment temperature stirs 40min to 25 DEG C, the ammonium persulfate aqueous solution 0.5kg for plus 1% and
5% aqueous solution of sodium bisulfite 0.5kg triggers, and rises to after maximum temperature, insulation reaction 1h, and PAMA is made
Reversed-phase emulsion finished product, the half that total amount is released afterwards is used as product.
Product can continuously be obtained by repeating the 3rd step and the 4th step.
Example three
The first step：40wt% acrylamide aqueous solution 750kg is sequentially added in 3000 liters of batching kettle, is added
With the sodium hydrate aqueous solution that mass concentration is 20% under the conditions of 125kg 2- acrylamide-2-methylpro panesulfonic acids, ice-water bath
The pH value of regulating system is 5.0.Emolsifier span 40 (Arlacel-20) 75kg and OP-10 25kg are added, are stirred
Mix after 30min, add hexamethylene 750kg,
Second step：It will be added to after the reversed-phase emulsion prepared of the first step in 5000 liters of polymeric kettles, adjust 15 DEG C of temperature, simultaneously
Logical high pure nitrogen stirs 40min with the oxygen in removing system.The ammonium persulfate aqueous solution 0.5kg's and 5% for plus 1% afterwards
Aqueous solution of sodium bisulfite 0.5kg is risen to after maximum temperature with triggering, insulation reaction 1h, PAMA is made anti-
Phase emulsion semi-finished product.
3rd step：40wt% acrylamide aqueous solution 1000kg is sequentially added in the batching kettle vacated, 125kg is added
It is for 20% sodium hydrate aqueous solution regulation with mass concentration under the conditions of 2- acrylamide-2-methylpro panesulfonic acids, ice-water bath
The pH value of system is 5.0, adds after 75kg the and OP-10 25kg of emolsifier span 40, stirring 30min, adds hexamethylene 750kg.
4th step：The reversed-phase emulsion that the 3rd step is prepared is added slowly to second step polyacrylamide under agitation anti-
In phase emulsion, lead to High Purity Nitrogen gas drive oxygen, adjustment temperature stirs 40min to 25 DEG C, the ammonium persulfate aqueous solution 0.5kg for plus 1% and
5% aqueous solution of sodium bisulfite 0.5kg triggers, and rises to after maximum temperature, insulation reaction 1h, and PAMA is made
Reversed-phase emulsion finished product, the half that total amount is released afterwards is used as product.
Product can continuously be obtained by repeating the 3rd step and the 4th step.
Claims (2)
1. a kind of preparation method of reversed phase latex of polyacrylamide, it is characterized in that comprising the following steps：
(1) acrylamide aqueous solution that mass concentration is 30-50% is sequentially added in the batching kettle with agitator, addition accounts for third
Acrylamide monomer mass 0-5% anhydrous sodium acetate, then account for acrylamide mole 0- by required anion degree addition
The sodium hydrate aqueous solution that 50% acrylic acid or 2- acrylamide-2-methylpro panesulfonic acids is 10-50% with mass concentration is adjusted
The pH value of section system is 3-7, adds this certain proportion of disk class emulsifying agent and octylphenol polyethylene for accounting for monomer gross mass 8-30%
Oxygen vinethene (OP) series emulsifying agent, opens stirring, until reactant is well mixed；Then add and account for acrylamide aqueous solution body
Product 60-120% organic solvent；
(2) reversed-phase emulsion for obtaining step (1) in batching kettle is added to enters equipped with agitator, thermometer, condenser and gas
In the polymeric kettle of outlet, lead to nitrogen or carbon dioxide flooding oxygen, it is 5-35 DEG C control temperature, stirring 30-60min, chemistry initiation or
Ultraviolet light initiated polymerization, reaction obtains reversed phase latex of polyacrylamide semi-finished product after terminating；
(3) this step is identical with step (1), and the total amount of dispensing releases the total of reversed phase latex of polyacrylamide product for step (4)
Amount；
(4) reversed-phase emulsion for preparing step (3) in batching kettle in whipping process is added slowly to the polypropylene in step (2)
In acid amides reversed-phase emulsion product, lead to nitrogen or carbon dioxide flooding oxygen, it is 5-35 DEG C to control temperature, stirs 30-60min, and chemistry draws
Hair or ultraviolet light initiated polymerization, reaction obtain reversed phase latex of polyacrylamide finished product after terminating；It is big according to reactor
Small and radiating efficiency, calculates or is drawn by experiment the optimised quantity for releasing product after reaction every time, release corresponding polypropylene
Acid amides reversed-phase emulsion product, releases the reversed phase latex of polyacrylamide product for accounting for 0.3-0.7 times of total amount.
2. the preparation method of a kind of reversed phase latex of polyacrylamide according to claim 1, it is characterized in that step (1) and step
Suddenly in (3), organic solvent is one kind in kerosene, atoleine, solvent naphtha or hexamethylene；This disk class emulsifying agent be this disk 20,
One kind in this disk 40, this disk 60, span 80 or this disk 85；OPEO (OP) series emulsifying agent is OP-4, OP-
6th, one kind in OP-8, OP-10, OP-15, OP-20 or OP-30.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710547581.4A CN107226875A (en) | 2017-07-06 | 2017-07-06 | A kind of preparation method of reversed phase latex of polyacrylamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710547581.4A CN107226875A (en) | 2017-07-06 | 2017-07-06 | A kind of preparation method of reversed phase latex of polyacrylamide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107226875A true CN107226875A (en) | 2017-10-03 |
Family
ID=59955999
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710547581.4A Pending CN107226875A (en) | 2017-07-06 | 2017-07-06 | A kind of preparation method of reversed phase latex of polyacrylamide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107226875A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104231162A (en) * | 2013-06-17 | 2014-12-24 | 中国石油化工股份有限公司 | Polyacrylamide reversed-phase microemulsion and preparation method thereof |
-
2017
- 2017-07-06 CN CN201710547581.4A patent/CN107226875A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104231162A (en) * | 2013-06-17 | 2014-12-24 | 中国石油化工股份有限公司 | Polyacrylamide reversed-phase microemulsion and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 地木拉提等: "丙烯酰胺反相乳液聚合的研究", 《新疆石油学院学报》 * |
| 许明标等: "《聚合物在油气田开采中的应用》", 31 January 2010, 中国地质大学出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Paquet Jr et al. | Tubular reactors for emulsion polymerization: I. Experimental investigation | |
| DE1240286B (en) | Process for the continuous emulsion polymerization of olefinically unsaturated compounds | |
| CN105085802B (en) | The synthetic method of hydrophobically modified polyacrylamide | |
| CN103894137B (en) | A kind of high shear reactor and the application in suspension polymerisation polyethylene glycol oxide is produced thereof | |
| CA1258334A (en) | Multi-modal emulsions of water-soluble polymers | |
| CN103554359A (en) | Method for preparing high-solid low-cost polyacrylamide reversed-phase microemulsion | |
| CN102336857B (en) | SAN (Styrene Acrylonitrile) resin with high nitrile content and narrow distribution and preparation method thereof | |
| CN108690155A (en) | The method that polyacrylamide is prepared by acrylamide using microreactor | |
| EP3307792B1 (en) | Method for producing vinyl acetate-ethylene copolymers by means of emulsion polymerization | |
| CN101205271A (en) | Method for producing PVC paste resin by employing composite emulsifier | |
| CA2390505C (en) | Emulsion polymerization process and reactor for such a process | |
| CN111704694B (en) | Continuous production process and continuous production device of emulsion type polymer and application thereof | |
| US4603154A (en) | Method for preparing dilute polymer solutions | |
| CN107226875A (en) | A kind of preparation method of reversed phase latex of polyacrylamide | |
| JPH069222A (en) | Continuous preparation of antimony pentaoxide | |
| US1896491A (en) | Process for emulsifying diolefines and for the production of products similar to latex | |
| US4464509A (en) | Apparatus and method for preparing polymers | |
| JPS58157801A (en) | Manufacture of water-in-oil emulsion of water-soluble polymer | |
| US4576978A (en) | Method for preparing polymer solutions | |
| US4508858A (en) | Apparatus and method for preparing polymer solutions | |
| CN105237679A (en) | Preparation method of oil well cement emulsion polymer fluid loss agent | |
| US4559202A (en) | Apparatus for preparing polymer solutions | |
| CN101519471A (en) | Emulsion-polymerizing preparation method of chlorinated polyether resin | |
| CN107474177A (en) | A kind of copolymerization composition manufacture method of calcium ions modified anion polyacrylamide | |
| CN103803747B (en) | Integrated high-efficiency water processing reactor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171003 |