CN109012483A - A kind of macromolecule emulsifier and preparation method thereof - Google Patents
A kind of macromolecule emulsifier and preparation method thereof Download PDFInfo
- Publication number
- CN109012483A CN109012483A CN201810570129.4A CN201810570129A CN109012483A CN 109012483 A CN109012483 A CN 109012483A CN 201810570129 A CN201810570129 A CN 201810570129A CN 109012483 A CN109012483 A CN 109012483A
- Authority
- CN
- China
- Prior art keywords
- parts
- emulsifier
- macromolecule
- macromolecule emulsifier
- acrylic
- 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
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
-
- 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
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
-
- 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
-
- 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
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
-
- 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
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1806—C6-(meth)acrylate, e.g. (cyclo)hexyl (meth)acrylate or phenyl (meth)acrylate
-
- 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
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1808—C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate
-
- 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
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1809—C9-(meth)acrylate
-
- 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
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1818—C13or longer chain (meth)acrylate, e.g. stearyl (meth)acrylate
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Polymerisation Methods In General (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of macromolecule emulsifiers and preparation method thereof, belong to polymeric material field.Above-mentioned macromolecule emulsifier includes following parts by weight of component: 10-70 parts of acrylic monomer, 5-50 parts of acrylic ester monomer, 0.01-5 parts of emulsifier, 1-10 parts of initiator, 1-40 parts of alkali, 50-200 parts of water；The acrylic monomer and acrylic ester monomer weight ratio are 1-7:1-5.The present invention is used in conjunction with by acrylic monomer, acrylic ester monomer and particular emulsifier, so that having good package action to mineral oil, vegetable oil, benzene class oil, emulsifying effectiveness is good with the alkyl chain of long-chain in the macromolecule emulsifier of preparation.Macromolecule emulsifier synthesis technology is simple, environmentally protective.
Description
Technical field
The present invention relates to polymeric material field, a kind of macromolecule emulsifier and preparation method thereof is particularly related to.
Background technique
Emulsifier is to prepare emulsion and assign substance used in its minimum stability, is essential group
Point.Common emulsifier is small-molecular emulsifier, mainly there is the nonionics such as alkyl phenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether
Emulsifier, the anion emulsifiers such as alkylbenzene sulfonate.Macromolecule emulsifier generally refers to relative molecular mass more than thousands of,
High-molecular compound with surface active function.By sources high molecular surfactant compound can be divided into natural polymer
Sub- surfactant, natural modified (or semi-synthetic) high molecular surfactant and chemical synthesis high-molecular surface active
Agent.Natural polymeric surface active agent is present in animal and plant body, and considerable effect is played in life process, be from
Amphipathy macromolecule compound prepared by animals and plants separation, purification；Modified high-molecular surfactant includes modified starch, fibre
Dimension element, protein and chitosan etc., i.e., using natural materials as primary raw material, obtain by working process；Synthesize macromolecule
Surfactant refers to hydrophilic monomer homopolymerization or is copolymerized with hydrophobic monomer, or passes through and pass through some common macromolecules
Chemical modification and be made, it is many kinds of, generally have polymeric type (polyacrylate etc.) and condensation class (such as polyamine).High score
Sub- emulsifier is the nearly 20 years a kind of New-type emulsifiers to grow up, is mainly developed by external trans-corporation, such as promise reputation, vapour bar
Transnational enterprise.Its production cycle is long, higher cost, is applied to the relatively high industry of product price, such as cosmetic industry more.Due to
It is limited by cost, it is seldom applied on pesticide industry.
It when Small molecular surfactant is as emulsifier, is adsorbed on oil/water interface as third phase, by reducing interface
Tension prevents dispersed phase drop poly-, obtains stable emulsion.However, surfactant emulsifies system is in metastable condition, belong to
Thermodynamic unstable system.Absorption of the surfactant on oil/water interface is a kind of dynamic equilibrium, under certain conditions,
Can be with quick adsorption and desorption, therefore have surfactant molecule and move to phenomenon in body phase, so as to cause the length of lotion
Phase stability is poor, and small molecule migration is also possible to bring many negative issues.Macromolecule emulsifier is since molecular weight is larger, tool
There is long oleophylic chain, can preferably wrap oily phase, stability can enhance.The synthetic method of macromolecule emulsifier has solution poly-
Conjunction, emulsion polymerization etc..Wherein polymerisation in solution will use a large amount of organic solvent, not environmentally；Emulsification used in emulsion polymerization
Agent is generally the compounding of small-molecular emulsifier, removes difficulty, influences performance.
Summary of the invention
The technical issues of to solve solvent used in macromolecule emulsifier synthesis and small-molecular emulsifier, the present invention provides
A kind of macromolecule emulsifier and preparation method thereof.
In order to solve the above technical problems, technical solution provided by the invention is as follows:
The present invention provides a kind of macromolecule emulsifier, is made of following parts by weight of component:
10-70 parts of acrylic monomer, 5-50 parts of acrylic ester monomer, 0.01-5 parts of emulsifier, macromolecule thickener,
1-10 parts of initiator, 1-40 parts of alkali, 50-200 parts of water；
Preferably, the equal relative molecular weight of macromolecule emulsifier weight is 10000-50000.
Preferably, the acrylic monomer is acrylic acid and/or methacrylic acid.
Preferably, the acrylic ester monomer be carbon number be the acrylate of 5-18 alcohol, carbon number is 5-18 alcohol
One or both of methacrylate.
Preferably, emulsifier is acrylate/C10-30 alkyl acrylate interlinkage copolymer；Specially trade name
For the commercial products of Pemulen TR-1, Pemulen TR-2.
Preferably, the alkali is sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, ammonium hydroxide, ethanol amine, diethyl
One or more of hydramine, triethanolamine.
The initiator is persulfate.
Preferably, the macromolecule emulsifier dosage accounts for the 3-15wt% of emulsification system.
The present invention also provides the preparations of above-mentioned polymeric acrylic acid esters macromolecule emulsifier, include the following steps:
Step 1: water, acrylic monomer, acrylic ester monomer, emulsifier, initiator are added to band according to weight
In the reaction kettle for having thermometer, shearing, stirring, condensation reflux unit, emulsification pretreatment 10min；
Step 2: temperature is slowly increased to 80-100 DEG C, reacts 2-6 hours；
Step 3: alkali neutralization is added, cooling, blowing.
Compared with prior art, the beneficial effects of the present invention are:
1. the present invention passes through additional proportion, the esters of acrylic acid carbochain of control acrylic monomer and acrylic ester monomer
Length adjust the HLB value of emulsifier, it is simple and convenient, assign the emulsifier excellent performance；
2. the present invention uses acrylate/C10-30 alkyl acrylate interlinkage copolymer as emulsifier, can not only make
System emulsification very well, and itself is exactly macromolecule emulsifier, will not bring other influences；
3. the present invention passes through acrylic monomer, acrylic ester monomer and acrylate/C10-30 alkyl acrylate
Interlinkage copolymer is used in conjunction with, so that with the alkyl chain of long-chain in the macromolecule emulsifier of preparation, to mineral oil, plant
Oil, benzene class oil have good package action, and emulsifying effectiveness is good；
4. present invention process synthesis is simple, environmentally protective.
Specific embodiment
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, specific embodiment will be used below
It is described in detail, but the present invention is limited to absolutely not these examples.The following is only the preferred embodiment of the present invention, is only used to
Explain the present invention, it cannot be construed as a limitation to the scope of the present invention.It should be pointed out that all of the invention
Any modifications, equivalent replacements, and improvements etc. done within spirit and principle, should all be included in the protection scope of the present invention.
Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
The present invention provides a kind of macromolecule emulsifier and preparation method thereof, and specific embodiment is as follows.
Embodiment 1:
A kind of macromolecule emulsifier is made of following parts by weight of component:
35 parts of acrylic acid, 35 parts of octadecyl acrylate, TR-10.5 parts of Pemulen, 3 parts of ammonium persulfate, sodium hydroxide 20
Part, 100 parts of water.
Preparation method includes:
Step 1: water, acrylic acid, octadecyl acrylate, Pemulen TR-1, ammonium persulfate are added to band according to weight
In the reaction kettle for having thermometer, shearing, stirring, condensation reflux unit, emulsification pretreatment 10min；
Step 2: temperature is slowly increased to 90 DEG C, reacts 4 hours；
Step 3: sodium hydroxide is added and neutralizes, cooling, blowing.
It is 33700 through the GPC detection equal relative molecular weight of macromolecule emulsifier weight.
Embodiment 2:
Octadecyl acrylate in embodiment 1 is changed to amyl acrylate, other are constant.
It is 37400 through the GPC detection equal relative molecular weight of macromolecule emulsifier weight.
Embodiment 3:
Octadecyl acrylate in embodiment 1 is changed to hexyl methacrylate, other are constant.
It is 36500 through the GPC detection equal relative molecular weight of macromolecule emulsifier weight.
Embodiment 4:
Octadecyl acrylate in embodiment 1 is changed to Isooctyl acrylate monomer, other are constant.
It is 38100 through the GPC detection equal relative molecular weight of macromolecule emulsifier weight.
Embodiment 5:
Octadecyl acrylate in embodiment 1 is changed to nonyl acrylate, other are constant.
It is 39400 through the GPC detection equal relative molecular weight of macromolecule emulsifier weight.
Embodiment 6:
Octadecyl acrylate in embodiment 1 is changed to lauryl methacrylate, other are constant.
It is 40300 through the GPC detection equal relative molecular weight of macromolecule emulsifier weight.
Embodiment 7:
Octadecyl acrylate in embodiment 1 is changed to Tridecyl methacrylate base ester, other are constant.
It is 35700 through the GPC detection equal relative molecular weight of macromolecule emulsifier weight.
Embodiment 8:
Octadecyl acrylate in embodiment 1 is changed to hexadecyl metrhacrylate, other are constant.
It is 34600 through the GPC detection equal relative molecular weight of macromolecule emulsifier weight.
Embodiment 9:
A kind of macromolecule emulsifier is made of following parts by weight of component:
10 parts of methacrylic acid, 50 parts of octadecyl acrylate, TR-10.01 parts of Pemulen, 5 parts of ammonium persulfate, hydroxide
1 part of potassium, 50 parts of water.
Preparation method includes:
Step 1: water, methacrylic acid, octadecyl acrylate, Pemulen TR-1, ammonium persulfate are added according to weight
Into the reaction kettle for having thermometer, shearing, stirring, condensation reflux unit, emulsification pretreatment 10min；
Step 2: temperature is slowly increased to 80 DEG C, reacts 6 hours；
Step 3: potassium hydroxide is added and neutralizes, cooling, blowing.
It is 38600 through the GPC detection equal relative molecular weight of macromolecule emulsifier weight.
Embodiment 10:
A kind of macromolecule emulsifier is made of following parts by weight of component:
10 parts of methacrylic acid, 5 parts of octadecyl acrylate, TR-22 parts of Pemulen, 1 part of ammonium persulfate, potassium hydroxide 10
Part, 90 parts of water.
Preparation method includes:
Step 1: water, methacrylic acid, octadecyl acrylate, Pemulen TR-2, ammonium persulfate are added according to weight
Into the reaction kettle for having thermometer, shearing, stirring, condensation reflux unit, emulsification pretreatment 10min；
Step 2: temperature is slowly increased to 100 DEG C, reacts 2 hours；
Step 3: potassium hydroxide is added and neutralizes, cooling, blowing.
It is 11400 through the GPC detection equal relative molecular weight of macromolecule emulsifier weight.
Embodiment 11:
A kind of macromolecule emulsifier is made of following parts by weight of component:
20 parts of methacrylic acid, 50 parts of octadecyl acrylate, TR-26 parts of Pemulen, 4 parts of ammonium persulfate, sodium carbonate 25
Part, 150 parts of water.
Preparation method includes:
Step 1: water, methacrylic acid, octadecyl acrylate, Pemulen TR-2, ammonium persulfate are added according to weight
Into the reaction kettle for having thermometer, shearing, stirring, condensation reflux unit, emulsification pretreatment 10min；
Step 2: temperature is slowly increased to 100 DEG C, reacts 2 hours；
Step 3: sodium carbonate is added and neutralizes, cooling, blowing.
It is 38400 through the GPC detection equal relative molecular weight of macromolecule emulsifier weight.
Embodiment 12:
A kind of macromolecule emulsifier is made of following parts by weight of component:
30 parts of acrylic acid, 40 parts of methacrylic acid, 20 parts of octadecyl acrylate, 30 parts of Tridecyl methacrylate base ester,
TR-16 parts of Pemulen, TR-24 parts of Pemulen, 10 parts of ammonium persulfate, 40 parts of sodium hydroxide, 200 parts of water.
Preparation method includes:
Step 1: by water, acrylic acid, methacrylic acid, octadecyl acrylate, Tridecyl methacrylate base ester,
Pemulen TR-1, Pemulen TR-2, ammonium persulfate are added to according to weight with thermometer, shearing, stirring, condensing reflux
In the reaction kettle of device, emulsification pretreatment 10min；
Step 2: temperature is slowly increased to 100 DEG C, reacts 2 hours；
Step 3: sodium hydroxide is added and neutralizes, cooling, blowing.
It is 50100 through the GPC detection equal relative molecular weight of macromolecule emulsifier weight.
Since length is limited, beneficial effect in order to further illustrate the present invention constructs following only by taking embodiment 1 as an example
Comparative example.
Comparative example 1:
Change the acrylic acid in embodiment 1 into octadecyl acrylate, other are constant.
Comparative example 2:
Change the octadecyl acrylate in embodiment 1 into acrylic acid, other are constant.
Comparative example 3:
Change the Pemulen TR-1 in embodiment 1 into lauryl sodium sulfate, other are constant.
Comparative example 4:
Octadecyl acrylate in embodiment 1 is changed to methyl acrylate, other are constant.
Comparative example 5:
Octadecyl acrylate in embodiment 1 is changed to Behenyl acrylate, other are constant.
Comparative example 6:
35 parts of octadecyl acrylate in embodiment 1 are reduced to 3 parts, other are constant.
Comparative example 7:
35 parts of acrylic acid in embodiment 1 are reduced to 5 parts, other are constant.
Comparative example 8:
Pemulen TR-1 in embodiment 1 is removed, other are constant.
Emulsifiability test is carried out to macromolecule emulsifier prepared by above-described embodiment 1-12 and comparative example 1-8, specifically such as
Under.
1. macromolecule emulsifier prepared by embodiment 1 is added to the water by the certain proportion of oil, it is made into 40% lotion, is used
Shearing emulsifier shears 5min, static 30min, observes stability of emulsion, the results are shown in Table 1.
1 stability of emulsion of table
As seen from the above table, when macromolecule emulsifier additive amount prepared by the present invention is 3% or more, the property of the lotion of preparation
It can be relatively stable.
2. the emulsifiability of the emulsifier of the macromolecule emulsifier and comparative example 1-8 preparation of pair above-described embodiment 1-12 preparation
It is detected.
(1) emulsifier estimation of stability
To 50mL mentioned emulsifier is added in desk centrifuge (TDZ5-WS) centrifuge tube, with the speed of 3000r/min from
Heart 30min, if stability is good, on the contrary then stability is poor without layering, without precipitating；
(2) stability of emulsion is evaluated
By above-mentioned macromolecule emulsifier 5%, fatty acid methyl ester 40%, water 55% is mixed in proportion, is cut with shearing emulsifier
5min is cut, lotion is made into.Stability of emulsion test is carried out according to GB/T 1603-2001 pesticidal emulsion stability, dilutes 100 times；
With D [V, 50] partial size of Mastorsizer2000 laser particle analyzer test lotion.Correlated performance is shown in Table 2.
Table 2
As shown in Table 2, lamination will not occur under the conditions of high speed centrifugation for macromolecule emulsifier prepared by the present invention, surely
It is qualitative preferable.Using the emulsifier fatty acid methyl ester, good emulsion stability, D [V, 50] partial size is smaller.By comparative example 1-8
It is found that the acrylic acid that the additional proportion of acrylic monomer and acrylic ester monomer is between 1-7:1-5, carbon number is 5-18 alcohol
The macromolecule emulsifier stability and emulsifiability of ester preparation are preferable；Pass through acrylic monomer, acrylic ester monomer and third
Olefin(e) acid ester/C10-30 alkyl acrylate interlinkage copolymer is used in conjunction with, so that having length in the macromolecule emulsifier of preparation
The alkyl chain of chain, emulsifying effectiveness are good.
3. the raising lotion of the emulsifier of the macromolecule emulsifier and comparative example 1-8 preparation of pair above-described embodiment 1-12 preparation
High-temperature stability test.
By above-mentioned macromolecule emulsifier 3%, OP-102%, fatty acid methyl ester 40%, water 55% mixes in proportion, with shearing
Emulsifier shears 5min.Sample is packed into ampoule bottle closure, is placed in 54 DEG C of insulating box and places for 24 hours, observation variation.With
D [V, 50] partial size of Mastorsizer2000 laser particle analyzer test heat storage front and back lotion.
Control treatment: by OP-105%, fatty acid methyl ester 40%, water 55% mixes in proportion, is sheared with shearing emulsifier
5min.Sample is packed into ampoule bottle closure, is placed in 54 DEG C of insulating box and places for 24 hours, observation variation.With
D [V, 50] partial size of Mastorsizer2000 laser particle analyzer test heat storage front and back lotion.
D [V, 50] partial size of control treatment heat storage front and back is respectively 1.0 μm, 25.4 μm, is darkened.Embodiment 1-12 and
The test result of comparative example 1-80 is shown in Table 3.
Table 3
Macromolecule emulsifier prepared by the present invention can be improved the high-temperature stability of lotion it can be seen from the above results,
The shortcomings that reducing low molecule emulsifier non-refractory.By comparative example 1-8 it is found that acrylic monomer and acrylic ester monomer
Additional proportion is between 1-7:1-5, carbon number interlinks for acrylate and acrylate/C10-30 alkyl acrylate of 5-18 alcohol
Copolymer is used in conjunction with the macromolecule emulsifier better stability of preparation.
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, it can also make several improvements and retouch, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of macromolecule emulsifier, which is characterized in that formed including following parts by weight of component:
10-70 parts of acrylic monomer, 5-50 parts of acrylic ester monomer, 0.01-5 parts of emulsifier, 1-10 parts of initiator, alkali 1-
40 parts, 50-200 parts of water；
The acrylic monomer and acrylic ester monomer weight ratio are 1-7:1-5.
2. macromolecule emulsifier according to claim 1, which is characterized in that the equal average molecular of the macromolecule emulsifier weight
Amount is 10000-50000.
3. macromolecule emulsifier according to claim 1, which is characterized in that the acrylic monomer be acrylic acid and/
Or methacrylic acid.
4. macromolecule emulsifier according to claim 1, which is characterized in that the acrylic ester monomer is that carbon number is 5-
One or both of the acrylate of 18 alcohol, methacrylate that carbon number is 5-18 alcohol.
5. macromolecule emulsifier according to claim 1, which is characterized in that the emulsifier is acrylate/C10-30
Alkyl acrylate interlinkage copolymer.
6. macromolecule emulsifier according to claim 5, which is characterized in that the acrylate/C10-30 alkyl
Acid esters interlinkage copolymer is specially the commercial products of trade name Pemulen TR-1, Pemulen TR-2.
7. macromolecule emulsifier according to claim 1, which is characterized in that the alkali is sodium hydroxide, potassium hydroxide, carbon
One or more of sour sodium, sodium bicarbonate, ammonium hydroxide, ethanol amine, diethanol amine, triethanolamine.
8. macromolecule emulsifier according to claim 1, which is characterized in that the initiator is persulfate.
9. -8 any macromolecule emulsifier according to claim 1, which is characterized in that the macromolecule emulsifier dosage accounts for
The 3wt% or more of emulsification system.
10. the preparation method of the described in any item macromolecule emulsifiers of claim 1-9, which comprises the steps of:
Step 1: water, acrylic monomer, acrylic ester monomer, emulsifier, initiator are added to band according to above-mentioned weight
In the reaction kettle for having thermometer, shearing, stirring, condensation reflux unit, emulsification pretreatment 10min；
Step 2: temperature is slowly increased to 80-100 DEG C, reacts 2-6 hours；
Step 3: alkali neutralization is added, cooling, blowing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810570129.4A CN109012483A (en) | 2018-06-05 | 2018-06-05 | A kind of macromolecule emulsifier and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810570129.4A CN109012483A (en) | 2018-06-05 | 2018-06-05 | A kind of macromolecule emulsifier and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109012483A true CN109012483A (en) | 2018-12-18 |
Family
ID=64612260
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810570129.4A Pending CN109012483A (en) | 2018-06-05 | 2018-06-05 | A kind of macromolecule emulsifier and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109012483A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111165477A (en) * | 2020-01-23 | 2020-05-19 | 中化化工科学技术研究总院有限公司 | Acetochlor emulsion in water and preparation method thereof |
| CN111269349A (en) * | 2020-01-23 | 2020-06-12 | 中化化工科学技术研究总院有限公司 | Polycarboxylic acid polymer emulsifier and preparation method thereof |
| CN111732719A (en) * | 2020-02-19 | 2020-10-02 | 江苏大学 | Preparation method of emulsifier based on polyhydroxy straight-chain polymer |
| CN114788792A (en) * | 2022-04-11 | 2022-07-26 | 苏州日月年世化妆品有限公司 | Preparation method of suspended microsphere composition |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1163279A (en) * | 1996-01-08 | 1997-10-29 | 巴斯福股份公司 | Preparation for non-soluble polymer |
| CN1621436A (en) * | 2003-11-26 | 2005-06-01 | 中国科学院成都有机化学有限公司 | Crosslinkable macromolecular emulsifier and its preparing process |
| US20070299180A1 (en) * | 2006-06-23 | 2007-12-27 | The Sherwin-Williams Company | High solids emulsions |
-
2018
- 2018-06-05 CN CN201810570129.4A patent/CN109012483A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1163279A (en) * | 1996-01-08 | 1997-10-29 | 巴斯福股份公司 | Preparation for non-soluble polymer |
| CN1621436A (en) * | 2003-11-26 | 2005-06-01 | 中国科学院成都有机化学有限公司 | Crosslinkable macromolecular emulsifier and its preparing process |
| US20070299180A1 (en) * | 2006-06-23 | 2007-12-27 | The Sherwin-Williams Company | High solids emulsions |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111165477A (en) * | 2020-01-23 | 2020-05-19 | 中化化工科学技术研究总院有限公司 | Acetochlor emulsion in water and preparation method thereof |
| CN111269349A (en) * | 2020-01-23 | 2020-06-12 | 中化化工科学技术研究总院有限公司 | Polycarboxylic acid polymer emulsifier and preparation method thereof |
| CN111269349B (en) * | 2020-01-23 | 2022-04-05 | 中化化工科学技术研究总院有限公司 | Polycarboxylic acid polymer emulsifier and preparation method thereof |
| CN111732719A (en) * | 2020-02-19 | 2020-10-02 | 江苏大学 | Preparation method of emulsifier based on polyhydroxy straight-chain polymer |
| CN114788792A (en) * | 2022-04-11 | 2022-07-26 | 苏州日月年世化妆品有限公司 | Preparation method of suspended microsphere composition |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109012483A (en) | A kind of macromolecule emulsifier and preparation method thereof | |
| CN108912277A (en) | A kind of polyacrylate macromolecule emulsifier and preparation method thereof | |
| AU2011361923A1 (en) | Method for thickening a cosmetic formulation using an alkali-swellable emulsion of an acrylic acid-rich AMPS polymer | |
| JP6889177B2 (en) | Microcapsules | |
| WO2017022702A1 (en) | Gel-form composition | |
| CN102858815A (en) | Polyacrylate (salt), polyacrylate (salt) water-absorbent resin, and manufacturing method for same | |
| CN106832112B (en) | A kind of self-dispersion type water-soluble cationic heavy crude thinner and preparation method thereof | |
| Chen et al. | Synthesis and properties of acrylic‐based superabsorbent | |
| AU2002337096B2 (en) | Inverter mixtures for polymer dispersions with improved environmental impact | |
| US2730498A (en) | Textile lubricants | |
| CN108659149B (en) | Fatty alcohol ester agricultural polymer emulsifier and preparation and use method thereof | |
| CN108883051B (en) | Gel composition, cosmetic, and method for producing gel composition | |
| CA2952180A1 (en) | Method for encapsulating oils in an aqueous medium with hase polymer emulsions, products obtained, and uses thereof | |
| CN105165846A (en) | BBIT water emulsion and preparation method thereof | |
| RU95107404A (en) | Addition agents to oil products and compositions | |
| CN102180996A (en) | Process for making uniform oligomeric droplets | |
| US5145914A (en) | Polyacrylate esters with ammonium salt groups | |
| CN111269349B (en) | Polycarboxylic acid polymer emulsifier and preparation method thereof | |
| CN108840996B (en) | Cardanol ester agricultural polymer emulsifier and preparation and use methods thereof | |
| ATE350403T1 (en) | POLYMER COMPOSITIONS CONTAINING MODIFIED POLYVINYL ALCOHOLS | |
| US20220267493A1 (en) | Thickened organic liquid compositions with polymeric rheology modifiers | |
| CA2237058A1 (en) | Copolymers of carboxylic acids and multiply olefinically unsaturated carboxylic acid derivatives and their use as thickeners and dispergents | |
| CN108990975A (en) | The agricultural macromolecule emulsifier of pine tar alkoxide and its preparation and application | |
| CN106318498A (en) | Biodiesel emulsifier, as well as preparation method and application thereof | |
| KR102634590B1 (en) | Droplets distributed in an aqueous medium |
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 |
Application publication date: 20181218 |
|
| RJ01 | Rejection of invention patent application after publication |