CN107973877A - A kind of copolymerization composition manufacture method of the polyacrylamide of modified anion containing magnesium ion - Google Patents
A kind of copolymerization composition manufacture method of the polyacrylamide of modified anion containing magnesium ion Download PDFInfo
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- CN107973877A CN107973877A CN201711335506.8A CN201711335506A CN107973877A CN 107973877 A CN107973877 A CN 107973877A CN 201711335506 A CN201711335506 A CN 201711335506A CN 107973877 A CN107973877 A CN 107973877A
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/16—Auxiliary treatment of granules
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- 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
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
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- Engineering & Computer Science (AREA)
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The present invention relates to a kind of copolymerization composition manufacture method of the polyacrylamide of modified anion containing magnesium ion.Its manufacture method is：Magnesium Acrylate Prepared solution is first prepared as raw material using acrylic acid and solid magnesium hydroxide or magnesia in batching kettle, below 20 DEG C, final solution pH value is controlled 6 to 8 whole reaction process temperature control；Then the solution to be polymerized that monomer mass concentration is 15% to 40% is made into for 95: 5 to 40: 60 chargings by the molar ratio of acrylamide and acrylic acid, cools down and add appropriate amount of addition agent, lead to nitrogen；Initiator, Continuous aeration to reaction solution is added to stop ventilation, closed polymeric kettle progress copolymerization after turning thick into polymeric kettle again；It is granulated, dried after complete reaction, being crushed, sieves packaging.Our forensic science is feasible, and raw materials are environmental-friendly, economic and practical, is adapted to large-scale industrial production, while the polyacrylamide of modified anion containing the magnesium ion performance produced is stable, molecular weight is high, accords with the demands of the market.
Description
Technical field
The invention belongs to the preparation field of anionic polyacrylamide, it is more particularly to a kind of containing magnesium ion be modified it is cloudy from
The copolymerization composition manufacture method of sub- polyacrylamide.
Background technology
Anionic polyacrylamide is all used widely in many fields, is that water-soluble polymer is most widely used
One of kind.It can be used as oil displacement agent, paper-making dispersant agent, flocculant, paper strengthening agent, drag reducer etc., be widely used in stone
The fields such as oily exploitation, drilling fracturing, papermaking, sewage disposal, coal.
Industrially the preparation method of anionic polyacrylamide mainly has three kinds, adds alkali homopolymerization before being respectively
Method, alkaline hydrolysis method and copolymerization process after homopolymerization.Preceding plus alkali homopolymerization method is before polymerization by acrylamide monomer and alkali
(generally sodium carbonate) while add in polymerization system, colloid is heated to more than 85 DEG C after polymerization in polymeric kettle
And keep the temperature 6 to 15 it is small when be hydrolyzed, then by granulating from colloid, drying, crush and screen to obtain final products.Add buck after homopolymerization
Solution is that acrylamide monomer and necessary auxiliary agent are comprised only in polymerization system, by granulating from colloid and then plus alkali after polymerization
(generally sodium hydroxide) is uniformly mixed, then heating hydrolysis, dry after hydrolysis, crush and screen to obtain final products.Combined polymerization
Method is in polymerization system while adds acrylamide monomer and the acrylic monomers with sum in sodium hydroxide, is incited somebody to action after polymerization
Colloid is directly granulated, dries, crushing and screening to obtain final products.From method made above can be seen that no matter which kind of method, most
The anionic polyacrylamide obtained eventually is all sodium ion to ion.
If magnesium ion will be changed over by sodium ion to ion in polymer, on the one hand in combined polymerization due to magnesium ion
Strong electrostatic screen reduces the electrostatic repulsion between anionic monomer, is conducive to obtain super high molecular weight product, on the other hand poly-
The viscosity of aqueous solution can be greatly lowered by closing the presence of magnesium ion in product, be met under many polyacrylamide use conditions,
Ask product that there is the molecular weight of superelevation, but the viscosity of aqueous solution wants alap requirement, while the introducing of magnesium ion can improve
Sensitiveness during polymer flocculation, improves flocculation ability.Chinese invention patent 201410678526.5 disclose it is a kind of containing magnesium from
Sub- modified polyacrylamide preparation method, obtained polymer are non-ionic, and organic solvent isopropyl is used in preparation process
Alcohol carries out precipitation process, and the method is not suitable for industrially mass producing.
The content of the invention
An object of the present invention is to provide a kind of anionic polyacrylamide being modified containing magnesium ion；
The second object of the present invention is to provide a kind of combined polymerization industry of anionic polyacrylamide being modified containing magnesium ion
Preparation method.
A kind of copolymerization composition manufacture method of anionic polyacrylamide being modified containing magnesium ion of the present invention includes following step
Suddenly：
1st, the preparation of Magnesium Acrylate Prepared solution：A certain amount of deionized water is added according to the volume size of kettle in batching kettle,
Then add acrylic acid, prepare the acrylic acid that mass concentration is 30%, cool to less than 20 DEG C, be slowly added and propylene
The solid magnesium hydroxide or magnesia of acid monomers equivalent, control whole process temperature are less than 20 DEG C, the pH value control of final solution
System obtains Magnesium Acrylate Prepared solution for later use in the range of 6 to 8.
2nd, the preparation of solution to be polymerized：Add a certain amount of deionized water first in another batching kettle, start stirring simultaneously
Cooling, acrylamide and above-mentioned steps (1) are added into batching kettle by the molar ratio 95: 5 to 40: 60 of acrylamide and acrylic acid
The Magnesium Acrylate Prepared solution of middle preparation, then add deionized water be configured to monomer mass concentration be 15% to 40% it is to be polymerized molten
Liquid, continues to cool down, and adds suitable auxiliary agent, and solution to be polymerized is transferred in polymeric kettle by temperature after reaching 0 DEG C to 8 DEG C, opens
Nitrogen switch is passed through nitrogen into polymeric kettle by throughput 1.0L/min.
3rd, combined polymerization：Into polymeric kettle, reaction solution continuously leads to nitrogen 30 minutes, while by greenhouse cooling to 0 DEG C to 8 DEG C, after
Initiator is added into polymeric kettle by certain time interval and carry out polymerisation, continue logical nitrogen to reaction solution after adding and turn
It is thick, stop logical nitrogen, closed polymeric kettle carries out copolymerization.
4th, it is granulated：Above-mentioned condensate is adiabatic reaction, therefore system constantly heats up in polymerization process, generally 1 to 10
Peak temperature is reached after hour, reaction system has been converted to colloidal at this time, continues held for some time to complete the reaction, reduces residual
Remaining content of monomer.Ventilate and pressurize into polymeric kettle superjacent air space, colloidal product is extruded into the screw rod through bottom at the same time from bottom
Comminutor be directly granulated to be adapted to drying magnitude range in, or bottom carry out preliminary granulation after through rotary knife comminutor be granulated to
It is adapted in dry magnitude range, installs a spraying device additional in pelletizer outlet, add dispersant, avoid in drying process
Mutual adhesion between particle.
5th, it is dry：Colloid product after granulation is delivered to the drying equipments such as rotary furnace or fluid bed to be dried, is controlled
Good drying temperature, makes product effective content >=85% of outflow drying equipment, and the product that drying equipment flows out is stored in feed bin
Inside it is cooled to room temperature.6th, crush, sieve packaging：The product cooled down in feed bin is delivered to disintegrating apparatus, after crushing on request
Granular size sieved, be then packaged into finished product.
The present invention copolymerization, in order to stablize properties of product, polymerisation need in certain pH value range into
OK, the polymerization reaction system pH value general control is in the range of 6 to 8.
The initial temperature general control of the copolymerization of the present invention is particularly controlled at 0 DEG C to 6 DEG C at 0 DEG C to 15 DEG C,
Polymerization rate is appropriate at this temperature, is conducive to obtain premium quality product.
Invention adds appropriate auxiliary agent in blending process, can play to adjust polymer molecular weight and change product and dissolve
The purpose of property.The auxiliary agent is one or more kinds of mixtures therein such as urea, thiocarbamide, disodium ethylene diamine tetraacetate.
The addition of the urea is the 0.1% to 5% of polymerized monomer gross mass, and the thiocarbamide addition is monomer gross mass
0.01% to 0.5%, the disodium ethylene diamine tetraacetate addition is the 0.1% to 2% of monomer gross mass.
The initiation system of the copolymerization of the present invention can be that single redox initiation system or redox add
The composite initiation system of azo.Oxidant in the initiation system is in persulfate, hydrogen peroxide, organic peroxy thing etc.
One or more kinds of mixtures.The persulfate is selected from sodium peroxydisulfate, ammonium persulfate, potassium peroxydisulfate etc..It is described
Organic peroxide can be tert-butyl hydroperoxide, t-butyl peroxy-acetate, methyl ethyl ketone peroxide, benzoyl peroxide
Deng one or both of thing mixed above.The reducing agent is sulphite, bisulfites, ferrous salt, trimethylamine
Deng.The sulphite is selected from ammonium sulfite, sodium sulfite, potassium sulfite etc., and the bisulfites is selected from sulfurous acid
Hydrogen ammonium, sodium hydrogensulfite, potassium bisulfite etc..The ferrous salt is green vitriol, six ferrous sulfate hydrate ammoniums, chlorine
Change ferrous iron etc..The trimethylamine is triethylamine, tetramethylethylenediamine, dimethylaminopropionitrile etc..The azo is selected from even
Nitrogen bis-isobutyronitrile, azobisisovaleronitrile, azobisisoheptonitrile, azo isobutyl cyano group formamide, azo diisopropyl imidazoline hydrochloride, azo
Two isobutyl dimethyl phthalates, azo-bis-isobutyrate hydrochloride, azo dicyano valeric acid etc..The addition of the oxidant is monomer
The 0.001% to 0.1% of quality, the addition of reducing agent are the 0.001% to 0.1% of monomer mass, and the addition of azo is
The 0.001% to 1% of monomer mass.
The present invention adds dispersant after granulating from colloid, and the dispersant is white oil, aviation kerosine or they and surface
The mixture of activating agent composition, the surfactant can be Span series such as Span60, Span65, Span80 etc., or
Polyoxyethylene ether series such as one or more kinds of mixtures therein such as OP-10, AEO-10.Dispersant addition is colloidal quality
The 1% to 5% of amount.
Embodiment
Embodiment 1：
In the batching kettle that volume is 10 cubic metres plus 4000kg deionized waters, 1200kg acrylic acid, stirring temperature control are less than
20 DEG C, 960kg magnesium hydroxides are slowly added into, reacting liquid pH value is adjusted after all dissolving in the range of 6 to 8.In another volume
, will be upper in 20 cubic metres of batching kettles plus deionized water 6300kg, acrylamide 800kg, to stir and cooling to less than 15 DEG C
State prepared Magnesium Acrylate Prepared solution to be transferred in this batching kettle, adjustment solution ph adds urea 100kg, thiocarbamide to 6.0
10kg, disodium ethylene diamine tetraacetate 40kg, dissolves and cools down, will be anti-after after all substances, all dissolving and temperature are reduced to 5 DEG C
Answer liquid to be transferred in polymeric kettle, open the logical nitrogen of nitrogen switch, after 30 minutes, prepared initiation in advance is added into reaction kettle
Agent, is respectively that ammonium persulfate 2kg is dissolved in 10kg deionized waters, and sodium sulfite 200g is dissolved in 10kg deionized waters, after
Continuous logical nitrogen turns thick to reaction solution, stops logical nitrogen, kettle is sealed, about 10 reach peak temperature when small, reaction solution becomes colloid, to kettle
Top blowing air pressurization extrudes colloid out of kettle, while is granulated through bottom screw pelletizer, and pelletizer outlet is per 1000kg
Colloid adds 50kg dispersants (No. 3 white oils), and colloid enters fluidized bed drying, dry postcooling to room temperature, then grinding screen subpackage
Dress up finished product.It is 19,000,000 by national standard detection molecules amount.
Embodiment 2：
As described in Example 1,13 side's reaction solutions are prepared, wherein monomer mass concentration is 40%, acrylamide and propylene
The molar ratio of acid is 95: 5, and adjustment solution ph adds urea 5kg to 8.0, thiocarbamide 500g, disodium ethylene diamine tetraacetate 5kg, molten
Solve and cool down, after all dissolving and temperature are reduced to 0 DEG C after all substances, reaction solution is transferred in polymeric kettle, opens nitrogen
The logical nitrogen of switch, after 30 minutes, prepared initiator in advance is added into reaction kettle, is respectively tert-butyl hydroperoxide 50g
It is dissolved in 10kg deionized waters, six ferrous sulfate hydrate ammonium 50g are dissolved in 10 deionization kg water, two NSC 18620 hydrochloric acid of azo
Salt 50kg is dissolved in 100kg deionized waters, is continued logical nitrogen to reaction solution and is turned thick, stops logical nitrogen, kettle is sealed, about 2 is small
When reach peak temperature, reaction solution becomes colloid, extrudes out of kettle colloid to blowing air pressurization above kettle, is granulated at the same time, comminutor
Exit adds 10kg dispersants (boat coal adds 5%Span60) by 1000kg colloids, and colloid enters fluidized bed drying, is cooled to room
Temperature, then crushes and screens and is packaged into finished product.It is 13,000,000 by national standard detection molecules amount.
Embodiment 3：
As described in Example 1,13 side's reaction solutions are prepared, wherein monomer mass concentration is 25%, acrylamide and propylene
The molar ratio of acid is 70: 30, and adjustment solution ph to 7.0, adds urea 30kg, disodium ethylene diamine tetraacetate 30kg, thiocarbamide 3kg,
Dissolve and cool down, after all dissolving and temperature are reduced to 8 DEG C after all substances, reaction solution is transferred in polymeric kettle, opens nitrogen
Air cock leads to nitrogen, and after 30 minutes, prepared initiator in advance is added into reaction kettle, is respectively potassium peroxydisulfate 1kg dissolvings
In 10kg water, sodium hydrogensulfite 20g is dissolved in 5kg water, and azodiisobutyronitrile 40g is dissolved in 10kg ethanol, continues to lead to
Nitrogen to reaction solution turns thick, stops logical nitrogen, kettle is sealed, and about 6 reach peak temperature when small, reaction solution becomes colloid, to kettle top
Blowing air pressurization extrudes colloid out of kettle, is granulated at the same time, and pelletizer outlet adds 30kg dispersants (boat coal by 1000kg colloids
Add 3%OP-10), colloid enters fluidized bed drying, is cooled to room temperature, and then crushes and screens and is packaged into finished product.By national standard detection point
Son amount is 20,000,000.
Embodiment 4：
As described in Example 1, dose volume is 13 cubic metres of reaction solution, and wherein monomer mass concentration is 20%, third
Acrylamide and the molar ratio of acrylic acid are 80: 20, and adjustment solution ph adds urea 50kg, disodium ethylene diamine tetraacetate to 7.5
3kg, thiocarbamide 15kg, dissolves and cools down, and all substances all dissolvings and after temperature is reduced to 3 DEG C, polymerization is transferred to by reaction solution
In kettle, the logical nitrogen of nitrogen switch is opened, after 30 minutes, prepared initiator in advance is added into reaction kettle, is respectively over cure
Sour ammonium 1kg is dissolved in 20kg water, and green vitriol 40g is dissolved in 5kg water, and azo-bis-isobutyrate hydrochloride 1kg is molten
Solution continues logical nitrogen to reaction solution and turns thick, stop logical nitrogen, kettle is sealed, about 5 reach peak temperature when small, reaction in 20kg water
Liquid becomes colloid, extrudes out of kettle colloid to blowing air pressurization above kettle, is granulated at the same time, pelletizer outlet presses 1000kg glue
Body adds 40kg dispersants (boat coal adds 1%AEO-10), and colloid enters fluidized bed drying, is cooled to room temperature, then grinding screen subpackage
Dress up finished product.It is 16,000,000 by national standard detection molecules amount.
Claims (1)
1. a kind of copolymerization composition manufacture method of the polyacrylamide of modified anion containing magnesium ion, it is characterised in that including following step
Suddenly：
(1) preparation of Magnesium Acrylate Prepared solution：A certain amount of deionized water is added according to the volume size of kettle in batching kettle, then
Acrylic acid is added, the acrylic acid that mass concentration is 30% is prepared, cools to less than 20 DEG C, be slowly added and acrylic acid list
The solid magnesium hydroxide or magnesia of body equivalent, control whole process temperature are less than 20 DEG C, and the pH value of final solution is controlled 6
To in the range of 8, Magnesium Acrylate Prepared solution for later use is obtained；
(2) preparation of solution to be polymerized：Start stirring and cool down, by the molar ratio 95: 5 to 40: 60 of acrylamide and acrylic acid
The Magnesium Acrylate Prepared solution prepared in acrylamide and above-mentioned steps (1) is added into batching kettle, then adds deionized water preparation
Into the solution to be polymerized that monomer mass concentration is 15% to 40%, continue to cool down, and add suitable auxiliary agent, temperature reaches 0 DEG C
Solution to be polymerized is transferred in polymeric kettle after to 8 DEG C, nitrogen switch is opened and nitrogen is passed through into polymeric kettle by throughput 1.0L/min
Gas；
(3) combined polymerization：Into polymeric kettle, reaction solution continuously leads to nitrogen 30 minutes, while greenhouse cooling is pressed afterwards to 0 DEG C to 8 DEG C
Certain time interval adds initiator into polymeric kettle and carries out polymerisation, continues logical nitrogen to reaction solution after adding and turns thick,
Stop logical nitrogen, closed polymeric kettle carries out copolymerization；
(4) it is granulated：Above-mentioned condensate is adiabatic reaction, therefore system constantly heats up in polymerization process, generally when 1 to 10 is small
Peak temperature is reached afterwards, and reaction system has been converted to colloidal at this time, continues held for some time to complete the reaction, reduces remaining single
Body content.Ventilate and pressurize into polymeric kettle superjacent air space, colloidal product is extruded the screw rod through bottom at the same time from bottom is granulated
Machine, which is directly granulated to, to be adapted in the magnitude range of drying, or is granulated after carrying out preliminary granulation in bottom through rotary knife comminutor to suitable
In dry magnitude range, install a spraying device additional in pelletizer outlet, add dispersant, avoid particle in drying process
Between mutual adhesion；
(5) it is dry：Colloid product after granulation is delivered to the drying equipments such as rotary furnace or fluid bed to be dried, is controlled dry
Dry temperature, makes outflow be stored in the product that drying equipment flows out cold in feed bin in product effective content >=85% of dry equipment
But to room temperature；
(6) crush, sieve packaging：The product cooled down in feed bin is delivered to disintegrating apparatus, the particle after crushing on request is big
It is small to be sieved, then it is packaged into finished product.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112707665A (en) * | 2019-11-19 | 2021-04-27 | 陕西科之杰新材料有限公司 | Aluminum sulfate alkali-free liquid accelerator and preparation method thereof |
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| CN1869088A (en) * | 2006-02-20 | 2006-11-29 | 四川大学 | Water soluble organic amphoteric high molecule copolymer and its preparation method |
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Application publication date: 20180501 |