CN107641167A - A kind of hydrophobically modified acrylic compounds association thickener and preparation method thereof - Google Patents
A kind of hydrophobically modified acrylic compounds association thickener and preparation method thereof Download PDFInfo
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- CN107641167A CN107641167A CN201710828828.XA CN201710828828A CN107641167A CN 107641167 A CN107641167 A CN 107641167A CN 201710828828 A CN201710828828 A CN 201710828828A CN 107641167 A CN107641167 A CN 107641167A
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Abstract
The invention discloses a kind of hydrophobically modified acrylic compounds association thickener and preparation method thereof, the thickener is prepared by the component of following parts by weight:30 60 parts of hydrophilic monomer, 20 70 parts of hydrophobic monomer, 0.5 10 parts of Hydrophobic association monomer, 5 15 parts of cross-linking monomer, 1.0 2.0 parts of emulsifying agent, 0.1 0.15 parts of initiator, 60 80 parts of solvent, its preparation method includes:(1) monomer emulsification prepares pre-emulsion;(2) preparation of initiator solution;(3) blend step (1) and the reaction solution of step (2) obtain hydrophobically modified acrylic compounds association thickener through emulsion polymerization, hydrophobically modified acrylic compounds association thickener provided by the invention can form the three-dimensional network polymer secondary structure using hydrophobic association body as net node, thickening effect and thixotropic property are excellent, with electrolyte-resistant ability, preparation method is simple and easy, is easy to industrialized production.
Description
Technical field
The present invention relates to new material the field of chemical synthesis, more particularly to a kind of hydrophobically modified acrylic compounds association thickener
And preparation method thereof.
Background technology
In recent years, water paint substitutes oil paint turns into trend of the times, during due to water paint to storage and construction
Viscosity requirement it is different, it is necessary to come regulation system viscosity and rheological property using thickener, during storage, remain high viscous
Degree, prevents cohesion and the precipitation of pigment, in painting process, by shear shinning, coating is had preferable brushability, brushes
After, lagged by of short duration viscosity, treat film levelling, viscosity recovery.By using thickener, coating height can be balanced and cut
Cut with low sheraing mobile performance, can both avoid storage during deposited phenomenon, also solve the problem that the levelling and stream during coating application
Extension problem, assign the good storage stability of coating and application property.
Polyacrylate-type thickeners are wide in variety because of its various structures, can meet the requirement of various rheological properties, be mesh
Preceding wide variety of a kind of thickener.Such thickener (UIG) is polymerized by 3 kinds or more of monomer at present, main monomer one
As be water-soluble monomer, as acrylic acid, maleic acid or maleic anhydride, methacrylic acid, acrylamide and 2- acrylamidos-
2- methyl propane sulfonic acid sodium etc.;Second comonomer is generally acrylate or styrene;Third monomer is the monomer for having crosslinked action,
Such as N,N methylene bis acrylamide, double acrylic acid fourth diester or diallyl phthalate etc..Polyacrylic thickens
The thickening mechanism of agent has neutralization thickening to thicken two kinds with Hydrogenbond.It is to use the agent for polyacrylic acid thickening of acidity to neutralize thickening
Alkali neutralizes, and makes its molecular ionization and produces negative electrical charge along the main chain of polymer, promotes by repelling each other between same sex electric charge
Strand, which stretches opening and forms network structure, reaches thickening effect.Hydrogenbond thickening is that polyacrylic acid molecule combines to form with water
Hydrate molecule, then pass through carboxylate radical as having the nonionic surfactant of 5 or more ethyoxyls to be combined with hydroxyl donor
The same sex electrostatic repulsion of ion, strand are stretched to bar-shaped by helical form, the strand of curling is solved open form in Aquo System
Reticulate structure and reach thickening effect.Inorganic electrolyte mass-energy significantly affects the thickening efficiency of such thickener, and monovalent ion can only
The thickening efficiency of reduction system, divalence or trivalent ion can not only make system thinning, and can be produced not when content is sufficiently high
Insoluble precipitate.Therefore, the electrolyte resistance of polycarboxylic acid thickener is very poor, it can not be answered in fields such as oil exploitations
With although the performance of its potential resistance to electrolyte contamination, this kind of thickening can be improved by adding the monomer containing sulfonic group etc. in thickener composition
Agent still suffers from many defects, such as the thixotropy of thickened systems is poor etc..
The content of the invention
For overcome the deficiencies in the prior art, an object of the present invention is that providing a kind of hydrophobically modified acrylic compounds forms
Thickener, by introducing hydrophobic long-chain side base in polymer chain structure, gained thickener has excellent thickening effect
And thixotropic property,
The second object of the present invention is to provide a kind of preparation side of above-mentioned hydrophobically modified acrylic compounds association thickener
Method, this method is simple and easy, is easy to industrialized production.
An object of the present invention adopts the following technical scheme that realization:
A kind of hydrophobically modified acrylic compounds association thickener, is prepared by the component of following parts by weight:
Further, one kind in itaconic acid, butene dioic acid, acrylic acid, methacrylic acid of the hydrophilic monomer or
It is two or more.
Further, the hydrophobic monomer is selected from styrene, vinylacetate, methyl acrylate, ethyl acrylate, propylene
It is more than one or both of propyl propionate, methacrylate.
Further, the Hydrophobic association monomer is selected from chain alkyl APEO acrylate, chain alkyl polyoxy
Ethene ether metacrylic acid ester, alkyl phenyl polyethylene oxides ether butenoate, triphenyl ethyl phenoxy ethers methacrylate
The C atomicities of middle one or more kinds of mixture, wherein chain alkyl are 16-25.
Further, the cross-linking monomer is selected from the double acrylic acid of divinylbenzene, diallyl phthalate, ethylene glycol
One kind in ester, glycol methacrylate, tirethylene glycol double methacrylate, tirethylene glycol double methyl methacrylate
It is or two or more.
Further, the emulsifying agent is selected from neopelex, lauryl sodium sulfate, OP-10, OP-21 mono-
Kind or two or more mixtures.
Further, the emulsifying agent is neopelex and OP10 with mass ratio 1:(1~2) mixing of combination
Thing.
Further, the initiator is selected from selected from one or both of ammonium persulfate, potassium peroxydisulfate or sodium peroxydisulfate
Mixture above.
Further, the solvent is water.
The second object of the present invention adopts the following technical scheme that realization:
The preparation method of above-mentioned hydrophobically modified acrylic compounds association thickener, comprises the following steps:
(1) monomer emulsification prepares pre-emulsion:60-80 parts solvent and 1.0-2.0 parts emulsifying agent are added in container, under stirring
30-60 part hydrophilic monomers, 20-70 parts hydrophobic monomer and 0.5-10 part Hydrophobic association monomers are added, then adds the crosslinking of 5-15 parts
Monomer, pre-emulsion is obtained after stirring 20-60min under 500-1000 revs/min of stir speed (S.S.);
(2) preparation of initiator solution:0.1-0.15 part initiators are dissolved in 10-50 part solvents, stirred, must be drawn
Send out agent solution;
(3) 4~6wt% and 100-150 part water of obtained pre-emulsion in step (1) are taken, is added together with 1.5-3.0 part emulsifying agents
Enter in reactor, stirred under 100-200 revs/min of stir speed (S.S.), be warming up to 70-90 DEG C, add 20wt% steps (2) preparation
Initiator solution, start to react;
(4) after reacting 20-30 minutes, the step of taking surplus pre-emulsion made from (1) and 60wt% steps (2) prepare
After initiator solution mixing, at the uniform velocity it is added drop-wise in the reactor of step (3), the step of adding surplus after being added dropwise to complete again (2)
Obtained initiator solution, 70-90 DEG C of reaction 1-2 hour, obtain hydrophobically modified acrylic compounds association thickener.
Compared with prior art, the beneficial effects of the present invention are:
1st, hydrophobically modified acrylic compounds association thickener provided by the invention can be formed using hydrophobic association body as net node
Three-dimensional network polymer secondary structure, thickening effect and thixotropic property are excellent;
2nd, hydrophobically modified acrylic compounds association thickener provided by the invention has electrolyte-resistant ability;
3rd, preparation method provided by the invention is simple and easy, is easy to industrialized production.
Embodiment
Below, with reference to embodiment, the present invention is described further, it is necessary to which explanation is, what is do not collided
Under the premise of, new embodiment can be formed between various embodiments described below or between each technical characteristic in any combination.
A kind of hydrophobically modified acrylic compounds association thickener, is prepared by the component of following parts by weight:Hydrophilic monomer
30-60 parts;Hydrophobic monomer 20-70 parts;Hydrophobic association monomer 0.5-10 parts;Cross-linking monomer 5-15 parts, emulsifying agent 1.0-2.0 parts;
Initiator 0.1-0.15 parts;Solvent 60-80 parts;Wherein, hydrophilic monomer is selected from itaconic acid, butene dioic acid, acrylic acid, metering system
Mixture more than one or both of acid, preferably acrylic or methacrylic acid;Hydrophobic monomer is selected from styrene, acetic acid
Mixing more than one or both of vinyl acetate, methyl acrylate, ethyl acrylate, propyl acrylate, methacrylate
Thing, preferably methyl acrylate or ethyl acrylate;Hydrophobic association monomer is selected from chain alkyl APEO acrylate, length
Alkyl group polyethenoxy ether metacrylic acid ester, alkyl phenyl polyethylene oxides ether butenoate, triphenyl ethyl phenoxy ethers first
The C atomicities of one or more kinds of mixture in base acrylate, wherein chain alkyl are 16-25, preferably long alkane
Base polyethenoxy ether metacrylic acid ester;Cross-linking monomer is selected from divinylbenzene, diallyl phthalate, ethylene glycol double third
In olefin(e) acid ester, glycol methacrylate, tirethylene glycol double methacrylate or tirethylene glycol double methyl methacrylate
One or more kinds of mixtures, preferably diallyl phthalate or glycol methacrylate;Emulsification
Agent is selected from mixture more than one or both of neopelex, lauryl sodium sulfate, OP-10 or OP-21,
It is preferred that neopelex and OP10 are with mass ratio 1:The mixture of 1-2 combinations;Initiator is selected from selected from ammonium persulfate, mistake
Mixture more than one or both of potassium sulfate or sodium peroxydisulfate, preferably sodium peroxydisulfate;Solvent is water.
The second object of the present invention adopts the following technical scheme that realization:
The preparation method of above-mentioned hydrophobically modified acrylic compounds association thickener, comprises the following steps:
(1) monomer emulsification prepares pre-emulsion:60-80 parts solvent and 1.0-2.0 parts emulsifying agent are added in container, under stirring
30-60 part hydrophilic monomers, 20-70 parts hydrophobic monomer and 0.5-10 part Hydrophobic association monomers are added, then adds the crosslinking of 5-15 parts
Monomer, pre-emulsion is obtained after stirring 20-60min under 500-1000 revs/min of stir speed (S.S.);
(2) preparation of initiator solution:0.1-0.15 part initiators are dissolved in 10-50 part solvents, stirred, must be drawn
Send out agent solution;
(3) 4-6wt% and 100-150 part water of obtained pre-emulsion in step (1) are taken, is added together with 1.5-3.0 part emulsifying agents
Enter in reactor, stirred under 100-200 revs/min of stir speed (S.S.), be warming up to 70-90 DEG C, add 20wt% steps (2) preparation
Initiator solution, start to react;
(4) after reacting 20-30 minutes, the step of taking surplus pre-emulsion made from (1) and 60wt% steps (2) prepare
After initiator solution mixing, at the uniform velocity it is added drop-wise in the reactor of step (3), the step of adding surplus after being added dropwise to complete again (2)
Obtained initiator solution, 70-90 DEG C of reaction 1-2 hour, obtain hydrophobically modified acrylic compounds association thickener.
Embodiment 1
(1) monomer emulsification prepares pre-emulsion:60 parts of (mass parts, similarly hereinafter) water and 1.0 parts of emulsifying agents are added in container, stirred
30 parts of acrylic acid of lower addition, 20 parts of methyl acrylates and 0.5 part of eicosyl polyethenoxy ether metacrylic acid ester are mixed, is then added
Enter 5 portions of diallyl phthalates, pre-emulsion is obtained after stirring 20min under 500 revs/min of stir speed (S.S.)s.
(2) preparation of initiator solution:0.1 part of sodium peroxydisulfate is dissolved in 10 parts of water, stirs, it is molten to obtain initiator
Liquid.
(3) obtained pre-emulsion 4wt% in step (1) is taken to be added together with 100 parts of water, 1.5 parts of emulsifying agents in reactor,
Stirred under 100 revs/min of stir speed (S.S.)s, be warming up to 70 DEG C, add the initiator solution of 20wt% steps (2) preparation, started
Reaction.
(4) after reacting 20min, by pre-emulsion made from (1) the step of surplus and the initiation of 60wt% steps (2) preparation
After agent solution mixing, at the uniform velocity it was added drop-wise in 3 hours in reactor, the step of adding surplus after adding again (2) is obtained to draw
Agent solution is sent out, 70 DEG C are reacted 1 hour, obtain hydrophobically modified acrylic compounds association thickener.
Wherein, emulsifying agent is neopelex and OP10 with mass ratio 1:1 mixture mixed.
Embodiment 2
(1) monomer emulsification prepares pre-emulsion:80 parts of water and 2.0 parts of emulsifying agents are added in container, stir lower 60 parts of addition
Methacrylic acid, 70 parts of ethyl acrylates and 10 parts of beheneth methacrylates, then add 15 parts of second
Ol dimethacrylate, pre-emulsion is obtained after stirring 60min under 1000 revs/min of stir speed (S.S.)s.
(2) preparation of initiator solution:0.15 part of sodium peroxydisulfate is dissolved in 50 parts of water, stirs, it is molten to obtain initiator
Liquid.
(3) obtained pre-emulsion 6wt% in step (1) is taken to be added together with 150 parts of water, 3.0 parts of emulsifying agents in reactor,
Stirred under 200 revs/min of stir speed (S.S.)s, be warming up to 90 DEG C, add the initiator solution of 20wt% steps (2) preparation, started
Reaction.
(4) after reacting 30min, by pre-emulsion made from (1) the step of surplus and the initiation of 60wt% steps (2) preparation
After agent solution mixing, at the uniform velocity it was added drop-wise in 3 hours in reactor, the step of adding surplus after adding again (2) is obtained to draw
Agent solution is sent out, 90 DEG C are reacted 2 hours, obtain hydrophobically modified acrylic compounds association thickener.
Wherein, emulsifying agent is neopelex and OP10 with mass ratio 1:2 mixtures mixed.
Embodiment 3
(1) monomer emulsification prepares pre-emulsion:70 parts of water and 1.5 parts of emulsifying agents are added in container, stir lower 50 parts of addition
Acrylic acid, 50 parts of ethyl acrylates and 2 parts of ceteth methacrylates, it is double then to add 10 parts of ethylene glycol
Methacrylate, pre-emulsion is obtained after stirring 30min under 800 revs/min of stir speed (S.S.)s.
(2) preparation of initiator solution:0.1 part of sodium peroxydisulfate is dissolved in 20 parts of water, stirs, it is molten to obtain initiator
Liquid.
(3) obtained pre-emulsion 5wt% in step (1) is taken to be added together with 120 parts of water, 2.0 parts of emulsifying agents in reactor,
Stirred under 150 revs/min of stir speed (S.S.)s, be warming up to 80 DEG C, add the initiator solution of 20wt% steps (2) preparation, started
Reaction.
(4) after reacting 30min, by pre-emulsion made from (1) the step of surplus and the initiation of 60wt% steps (2) preparation
After agent solution mixing, at the uniform velocity it was added drop-wise in 3 hours in reactor, the step of adding surplus after adding again (2) is obtained to draw
Agent solution is sent out, 80 DEG C are reacted 2 hours, obtain hydrophobically modified acrylic compounds association thickener.
Wherein, emulsifying agent is neopelex and OP10 with mass ratio 1:1 mixture mixed.
Embodiment 4
(1) monomer emulsification prepares pre-emulsion:60 parts of water and 2.0 parts of emulsifying agents are added in container, stir lower 40 parts of addition
Methacrylic acid, 60 parts of ethyl acrylates and 5 parts of pentacosyl polyethenoxy ether metacrylic acid esters, then add 12 parts of neighbours
Dially phthalate, pre-emulsion is obtained after stirring 30min under 500 revs/min of stir speed (S.S.)s.
(2) preparation of initiator solution:0.15 part of sodium peroxydisulfate is dissolved in 30 parts of water, stirs, it is molten to obtain initiator
Liquid.
(3) obtained pre-emulsion 5wt% in step (1) is taken to be added together with 120 parts of water, 2.0 parts of emulsifying agents in reactor,
Stirred under 100 revs/min of stir speed (S.S.)s, be warming up to 70 DEG C, add the initiator solution of 20wt% steps (2) preparation.Start
Reaction.
(4) after reacting 20min, by pre-emulsion made from (1) the step of surplus and the initiation of 60wt% steps (2) preparation
After agent solution mixing, at the uniform velocity it was added drop-wise in 3 hours in reactor, the step of adding surplus after adding again (2) is obtained to draw
Agent solution is sent out, 70 DEG C are reacted 1 hour, obtain hydrophobically modified acrylic compounds association thickener.
Wherein, emulsifying agent is neopelex and OP10 with mass ratio 1:1 mixture mixed.
Thickening property is tested:The thickener products adjustment that embodiment 1-4 is obtained is solid containing being 50%, takes 8g to be added to 200g benzene
In acrylic emulsion (ACRONAL 7035), it is 7.5 to adjust pH with ammoniacal liquor, stirs 20min, and the rotation that emulsion is tested after standing 20min sticks
Spend (NDJ-1 type rotational viscometers, 6rpm and 60rpm), and be not added with thickener products contrast, as a result as shown in table 1.
Viscosity and thixotropic index under the different shearings of table 1
What embodiment 1 to 4 synthesized as shown in Table 1 is used for hydrophobically modified acrylic compounds association thickener after measured, when it
When dosage is 2%, viscosity of the styrene-acrylic emulsion under the conditions of 6rpm can be made to increase to more than 3000cps from 152cps,
Viscosity under the conditions of 60rpm increases to more than 1200cps from 150cps, illustrates there is good thickening effect;Phenylpropyl alcohol breast
Viscosity ratio (thixotropic index) of the liquid under the conditions of 6rpm and 60rpm is more than 2.0, illustrates to be provided with preferable shear shinning
Effect.
Electrolyte-resistant is tested:The NaCl solution of various concentrations is added dropwise to the styrene-acrylic emulsion of above-mentioned addition thickener, stirring is equal
It is even and stand after 20min with the viscosity under the conditions of NDJ-1 types rotational viscometer test 6rpm, as a result as shown in table 2.
Viscosity under 2 different electrolyte concentrations of table
As can be seen from Table 2, after with the addition of electrolyte, thickening effect has declined, but in 0.3wt% electrolyte concentration
Under, viscosity remains to be maintained at more than 1000cps, illustrates there is preferable potential resistance to electrolyte contamination ability.
Above-mentioned embodiment is only the preferred embodiment of the present invention, it is impossible to the scope of protection of the invention is limited with this,
The change and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed scope.
Claims (10)
1. a kind of hydrophobically modified acrylic compounds association thickener, it is characterised in that be prepared by the component of following parts by weight:
A kind of 2. hydrophobically modified acrylic compounds association thickener according to claim 1, it is characterised in that the hydrophilic list
Body is selected from more than one or both of itaconic acid, butene dioic acid, acrylic acid, methacrylic acid.
A kind of 3. hydrophobically modified acrylic compounds association thickener according to claim 1, it is characterised in that the hydrophobic list
The one kind of body in styrene, vinylacetate, methyl acrylate, ethyl acrylate, propyl acrylate, methacrylate
It is or two or more.
4. a kind of hydrophobically modified acrylic compounds association thickener according to claim 1, it is characterised in that described hydrophobic to form
Close monomer and be selected from chain alkyl APEO acrylate, chain alkyl polyethenoxy ether metacrylic acid ester, alkyl phenyl
One or more kinds of mixture in APEO butenoate, triphenyl ethyl phenoxy ethers methacrylate, its
The C atomicities of middle chain alkyl are 16-25.
5. a kind of hydrophobically modified acrylic compounds association thickener according to claim 1, it is characterised in that the crosslinking is single
Body is selected from divinylbenzene, diallyl phthalate, ethylene glycol diacrylate, glycol methacrylate, two
It is more than one or both of condensed ethandiol double methacrylate, tirethylene glycol double methyl methacrylate.
A kind of 6. hydrophobically modified acrylic compounds association thickener according to claim 1, it is characterised in that the emulsifying agent
The mixture one or more kinds of selected from neopelex, lauryl sodium sulfate, OP-10, OP-21.
A kind of 7. hydrophobically modified acrylic compounds association thickener according to claim 6, it is characterised in that the emulsifying agent
It is neopelex and OP10 with mass ratio 1:(1~2) mixture of combination.
A kind of 8. hydrophobically modified acrylic compounds association thickener according to claim 1, it is characterised in that the initiator
Selected from the mixture more than one or both of ammonium persulfate, potassium peroxydisulfate or sodium peroxydisulfate.
9. a kind of hydrophobically modified acrylic compounds association thickener according to claim 1, it is characterised in that the solvent is
Water.
10. a kind of preparation method of the hydrophobically modified acrylic compounds association thickener as described in claim any one of 1-9, it is special
Sign is, comprises the following steps:
(1) monomer emulsification prepares pre-emulsion:60-80 parts solvent and 1.0-2.0 parts emulsifying agent are added in container, stir lower add
30-60 part hydrophilic monomers, 20-70 parts hydrophobic monomer and 0.5-10 part Hydrophobic association monomers, 5-15 part cross-linking monomers are then added,
Pre-emulsion is obtained after stirring 20-60min under 500-1000 revs/min of stir speed (S.S.);
(2) preparation of initiator solution:0.1-0.15 part initiators are dissolved in 10-50 part solvents, stirs, obtains initiator
Solution;
(3) 4-6wt% and 100-150 part water of obtained pre-emulsion in step (1) are taken, is added instead together with 1.5-3.0 part emulsifying agents
Answer in device, stirred under 100-200 revs/min of stir speed (S.S.), be warming up to 70-90 DEG C, add drawing for 20wt% steps (2) preparation
Agent solution is sent out, starts to react;
(4) after reacting 20-30 minutes, the step of taking surplus pre-emulsion made from (1) and the initiation for preparing of 60wt% steps (2)
After agent solution mixing, at the uniform velocity it is added drop-wise in the reactor of step (3), the step of adding surplus after being added dropwise to complete again (2) is made
Initiator solution, 70-90 DEG C reaction 1-2 hours, obtain hydrophobically modified acrylic compounds association thickener.
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CN111961212A (en) * | 2020-08-28 | 2020-11-20 | 浙江九本环保技术有限公司 | Novel rheological thickening water-retaining agent for papermaking, preparation method and application |
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