CN110407971A - A kind of pure phenylpropyl alcohol building emulsion and preparation method thereof - Google Patents
A kind of pure phenylpropyl alcohol building emulsion and preparation method thereof Download PDFInfo
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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
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
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- 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
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- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D125/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Coating compositions based on derivatives of such polymers
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- C09D141/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a bond to sulfur or by a heterocyclic ring containing sulfur; Coating compositions based on derivatives of such polymers
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Abstract
The present invention relates to a kind of pure phenylpropyl alcohol building emulsions and preparation method thereof, belong to styrene-acrylic emulsion technical field, its raw material includes water, composite emulsifier, n-butyl acrylate, styrene, acrylamide, acrylic acid, bottom solution, first initiator, reaction initiator, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution, oxidant, reducing agent, defoaming agent, fungicide, bottom solution includes water, reaction emulsifier, sodium bicarbonate, the weight proportion of n-butyl acrylate and styrene is 1:1, the mass fraction of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is 1.78%.The pure phenylpropyl alcohol building emulsion, not only solid content with higher, but also there is lower viscosity, while also having the advantages that lower partial size, and suitable for matt latex paint, satin emulsion.
Description
Technical field
The present invention relates to styrene-acrylic emulsion technical fields, more specifically, it be related to a kind of pure phenylpropyl alcohol building emulsion and its
Preparation method.
Background technique
Styrene-acrylic emulsion is to be obtained by styrene and Butyl Acrylate Monomer through emulsion copolymerization, and styrene-acrylic emulsion is in emulsion polymerization
Studying more system and the world today has one of ten big non-crosslinked type lotions of essential industry application value.Styrene-acrylic emulsion
As a kind of important intermediate chemical products, there is very extensive purposes, be now mainly used as building coating, metal surface latex
Coating, floor coating, paper adhesives, adhesive etc..Solid content is an important indicator of average styrene-acrylic emulsion, and solid content is
Remainder accounts for the mass percent of total amount after lotion or coating are dried under prescribed conditions, and the increase of solid content can effectively reduce
Drying time in use process, but while solid content increase, water is added in reaction and necessarily reduces, so as to cause lotion
Partial size increases, and reduces emulsion intercalation method, and also increase the viscosity of lotion, not only influences the stability of storage, Er Qieke
Being normally carried out for polymerization reaction can be influenced, therefore, is badly in need of studying the styrene-acrylic emulsion of a kind of high solids content, low viscosity, low partial size, with
Suitable for matt latex paint, satin emulsion.
Summary of the invention
The purpose of the present invention is to provide a kind of pure phenylpropyl alcohol building emulsion, not only solid content with higher, but also
Also there is lower viscosity, while also having the advantages that lower partial size, and suitable for matt latex paint, satin emulsion.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of pure phenylpropyl alcohol building emulsion, according to parts by weight, raw material include 700-1000 parts of water, composite emulsifier 6.5-10
Part, 855-1040 parts of n-butyl acrylate, 855-1040 parts of styrene, 34-50 parts of acrylamide, 22-34 parts of acrylic acid, bottom
846-1122 parts of solution, initiator 28-42 parts first, 120-180 parts of reaction initiator, methylacryoyloxyethyl trimethyl ammonia chloride
93-134 parts of ammonium salt solution, 13.2-19.8 parts of oxidant, 41-61 parts of reducing agent, 1.5-2.5 parts of defoaming agent, fungicide 1.5-2.5
Part, the bottom solution includes 800-1200 parts of water, 7.8-11 parts of reaction emulsifier, 1-1.4 parts of sodium bicarbonate, the acrylic acid
The weight proportion of N-butyl and styrene is 1:1, the mass fraction of the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution
It is 1.78%.
By using above-mentioned technical proposal, synergistic effect and n-butyl acrylate and styrene between each raw material
Weight proportion is 1:1, the mass fraction of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is 1.78%, builds pure phenylpropyl alcohol
Lotion not only solid content with higher is built, but also there is lower viscosity, while also having the advantages that lower partial size.
Preferably, raw material includes 750-900 parts of water, 7.5-9.2 parts of composite emulsifier, n-butyl acrylate 900-
968 parts, 900-968 parts of styrene, 39-46 parts of acrylamide, 25-30 parts of acrylic acid, solution 923-1084 parts of bottom, just initiation
32-39 parts of agent, 135-165 parts of reaction initiator, 108-134 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution, oxidation
14.8-18.1 parts of agent, 46.3-51.5 parts of reducing agent, 1.8-2.2 parts of defoaming agent, 1.8-2.2 parts of fungicide, the bottom solution
Including 900-1100 parts of water, 8.5-10.5 parts of reaction emulsifier, 1.1-1.3 parts of sodium bicarbonate.
By using above-mentioned technical proposal, the raw material proportioning of pure phenylpropyl alcohol building emulsion is optimized, is further increased
The solid content of pure phenylpropyl alcohol building emulsion, while further decreasing its viscosity.
Preferably, the just initiator is the ammonium persulfate solution that mass fraction is 18.33%, the reaction initiator
It is the ammonium persulfate solution that mass fraction is 4.14%.
By using above-mentioned technical proposal, the mass fraction of first initiator is defined, and makes to be formed in the solution of bottom
A certain amount of free radical avoids the amount of first initiator too small and reduces the number of free radical in the solution of bottom, and then influences subsequent
Raolical polymerizable, while also avoiding the amount of first initiator excessive and eliminating its own collision, to the matter of reaction initiator
Amount score is defined, and makes to be capable of forming metastable number of free radical in free radical polymerization system, to maintain radical polymerization
Close reaction efficiency, avoid the amount of reaction initiator too small and reduce reaction effect, also avoid the amount of reaction initiator excessive and
There is the case where itself collision is eliminated.
Preferably, the pH value of the pure phenylpropyl alcohol building emulsion controls between 7.5-9.
By using above-mentioned technical proposal, pure phenylpropyl alcohol building emulsion is made to be in alkaline condition, improves pure phenylpropyl alcohol and build
Build the stability of lotion storage.
Preferably, the composite emulsifier includes lauryl sodium sulfate, Value 3608, isomery ten
Alcohol polyoxyethylene ether, the allyloxy hydroxypropyl azochlorosulfonate acid sodium: Value 3608: heterogeneous ten alcohol polyoxyethylene ether
Weight proportion be 4:1.3:1.
By using above-mentioned technical proposal, composite emulsifier is optimized, by the synergistic effect between raw material, not only
The emulsifying effectiveness between raw material is improved, and also reduces the partial size of lotion, viscosity, so that pure phenylpropyl alcohol building emulsion be made to have
There is good performance.
Preferably, the reaction emulsifier is allyloxy hydroxypropyl azochlorosulfonate acid sodium.
By using above-mentioned technical proposal, allyloxy hydroxypropyl azochlorosulfonate acid sodium can be played as a kind of surfactant
Good emulsifying effectiveness makes n-butyl acrylate, styrene whens n-butyl acrylate, styrene etc. being added in the solution of bottom
It is come into full contact with the free radical in the solution of bottom, and causes Raolical polymerizable, to accelerate the reaction of free radical polymerization.
Preferably, it is 10% tert-butyl hydroperoxide solution that the oxidant, which is mass fraction, and the reducing agent is matter
Amount score is 3% rongalite solution.
By using above-mentioned technical proposal, to the reducing substances in tert-butyl hydroperoxide consumption raw material, rongalite disappears
The oxidation material in raw material is consumed, to improve the stability of pure phenylpropyl alcohol building emulsion, and pure phenylpropyl alcohol is also improved and builds
The inoxidizability of lotion is built, while passing through the mass fraction of mass fraction, rongalite solution to tert-butyl hydroperoxide solution
It is defined respectively, avoids the additional amount of oxidant, reducing agent very few and influence its using effect, also avoid oxidant, reduction
The additional amount of agent is excessive and increases its production cost.
The purpose of the present invention two is to provide a kind of method for preparing a kind of above-mentioned pure phenylpropyl alcohol building emulsion, passes through each original
The mutual cooperation between synergistic effect and each step between material, makes pure phenylpropyl alcohol building emulsion, not only with higher
Solid content, but also have the advantages that lower viscosity, low partial size.
Above-mentioned technical purpose of the invention has the technical scheme that
A method of a kind of above-mentioned pure phenylpropyl alcohol building emulsion is prepared, is included the following steps:
(1) water, reaction emulsifier, sodium bicarbonate are uniformly mixed, obtain bottom solution, it is spare；
(2) water, composite emulsifier, n-butyl acrylate, styrene, acrylamide, acrylic acid are uniformly mixed, it is single obtains mixing
Liquid solution, it is spare；
(3) under conditions of temperature is 83 DEG C, just initiator is added into bottom solution, then by the way of being added dropwise, respectively
Mixed monomer solution and reaction initiator is added dropwise, and controls temperature and is added dropwise at 86 DEG C, and in 2-4h, methyl is added later
Acrylyl oxy-ethyl-trimethyl salmiac solution, insulation reaction 1-3h；
(4) cool down most 70 DEG C, addition oxidant, insulation reaction 4-8min, addition reducing agent, insulation reaction 10-60min, it
Defoaming agent, fungicide are added afterwards, is uniformly mixed, obtains pure phenylpropyl alcohol building emulsion.
By using above-mentioned technical proposal, first initiator forms a certain amount of free radical in the solution of bottom, and reaction causes
Agent makes to maintain metastable number of free radical in Raolical polymerizable system, by between first initiator and reaction initiator
Synergistic effect, accelerate the efficiency of Raolical polymerizable, mixed monomer solution be added by the way of dropwise addition and reaction is drawn
Agent is sent out, more evenly, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution, methacryloxypropyl is then added in the mixing for making raw material
Polymerization reaction also occurs for ethyl-trimethyl salmiac and raw material, by synergistic effect between each raw material and each step it
Between mutual cooperation, make pure phenylpropyl alcohol building emulsion, not only solid content with higher, but also there is lower viscosity, low
The advantages of partial size, improves the steady of pure phenylpropyl alcohol building emulsion storage by the way that oxidant, reducing agent, defoaming agent, fungicide is added
It is qualitative.
Preferably, the pure phenylpropyl alcohol building emulsion adjusts pH value using ammonium hydroxide, and the mass fraction of the ammonium hydroxide is
5%.
By using above-mentioned technical proposal, the pH value of pure phenylpropyl alcohol building emulsion is adjusted using ammonium hydroxide, ammonium hydroxide raw material is easy to get,
Production cost is reduced, and the mass fraction of ammonium hydroxide is defined, adjusts the pH value of pure phenylpropyl alcohol building emulsion more convenient.
Preferably, just initiator, the reaction initiator are completed using preparation in preceding 30min, the methyl-prop
Alkene acyloxyethyl trimethyl ammonia chloride ammonium salt solution is completed using preparation in preceding 3min.
By using above-mentioned technical proposal, first initiator, reaction initiator after the completion of preparation, inside generate immediately it is few
The free radical of amount, and free radical has certain half-life period, limits the preparation deadline of first initiator, reaction initiator
It is fixed, it avoids the preparation time of first initiator, reaction initiator from reducing the free radical generated in it too early, also avoids just causing
Agent, reaction initiator the preparation time influence its use too late.MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is in length
It is dissolved in the case where time placement and is oxidized and changes colour, the preparation of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is completed
Time is defined, and the preparation time of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is avoided to make its own generation too early
Oxidation is reunited, to influence its using effect.
In conclusion the invention has the following advantages:
The first, the pure phenylpropyl alcohol building emulsion of the purpose of the present invention, not only solid content with higher, but also have lower
Viscosity, while also having the advantages that lower partial size.
The second, the mass fraction of first initiator, the mass fraction of reaction initiator are defined, not only increase and just draws
The using effect of agent, reaction initiator is sent out, and reduces production cost, while composite emulsifier, reaction emulsifier are carried out
Optimization, by the synergistic effect between raw material, not only increases the emulsifying effectiveness between raw material, and also reduce the grain of lotion
Diameter, viscosity, to keep pure phenylpropyl alcohol building emulsion with good performance.
Third, the method for preparing pure phenylpropyl alcohol building emulsion of the invention, by the synergistic effect between each raw material, and
Mutual cooperation between each step makes pure phenylpropyl alcohol building emulsion, not only solid content with higher, but also has lower
Viscosity, low partial size the advantages of.
4th, it is defined by the preparation time to first initiator, reaction initiator, improves just initiator, reaction
The stability and using effect that initiator uses pass through the preparation time to MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution
It is defined, improves the stability and using effect that MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution uses.
Specific embodiment
Invention is further described in detail with reference to embodiments.It should be understood that described in the embodiment of the present invention
Preparation method is only used for illustrating the present invention, rather than limiting the invention, to this hair under concept thereof of the invention
The simple modifications of bright preparation method belong to the scope of protection of present invention.
Each material content (unit: Kg) of bottom solution in 1 embodiment of table
| Bottom solution | One | Two | Three | Four | Five |
| Water | 800 | 900 | 1000 | 1100 | 1200 |
| Reaction emulsifier | 8.5 | 10.5 | 9.8 | 7.8 | 11 |
| Sodium bicarbonate | 1 | 1.3 | 1.2 | 1.1 | 1.4 |
Each material content (unit: Kg) of pure phenylpropyl alcohol building emulsion in 2 embodiment of table
Embodiment 1
A kind of pure phenylpropyl alcohol building emulsion, raw material proportioning are shown in Table 1, table 2；
(1) in mixing kettle, water, allyloxy hydroxypropyl azochlorosulfonate acid sodium reaction emulsifier, sodium bicarbonate is uniformly mixed, kettle is obtained
Bottom solution, it is spare；
(2) in another mixing kettle, by water, composite emulsifier, n-butyl acrylate, styrene, acrylamide, acrylic acid
It is uniformly mixed, the weight proportion of n-butyl acrylate and styrene is 1:1 at this time, obtains mixed monomer solution, spare；
(3) bottom solution is added in a kettle, and under conditions of temperature is 83 DEG C, adds in the bottom solution into reaction kettle
Enter just initiator, it is 18.33% ammonium persulfate solution that first initiator, which selects mass fraction, and just reaction kettle is being added in initiator
Preceding 30min, which is prepared, to be completed, and controls temperature at 86 DEG C, then by the way of being added dropwise, it is single that mixing is added dropwise into reaction kettle respectively
Liquid solution and reaction initiator, the ammonium persulfate solution that reaction initiator selection mass fraction is 4.14%, and reaction initiator
30min before reaction kettle is added, which is prepared, to be completed, and mixed monomer solution and reaction initiator are added dropwise in 2h, backward
The MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution that mass fraction is 1.78%, methacryloxypropyl second are added in reaction kettle
3min of the base trimethyl ammonia chloride ammonium salt solution before reaction kettle is added, which is prepared, to be completed, insulation reaction 3h；
(4) by most 70 DEG C of the greenhouse cooling in reaction kettle, oxidant is added, it is 10% tert-butyl that oxidant, which selects mass fraction,
Reducing agent is added in hydrogenperoxide steam generator, insulation reaction 5min, and it is 3% rongalite solution that reducing agent, which selects mass fraction, and heat preservation is anti-
45min is answered, polyoxyethylene polyoxy Propanolamine ether defoaming agent, Brassicol are added later, is uniformly mixed, obtains pure
Then greenhouse cooling in reaction kettle is used mass fraction to adjust its pH for 5% ammonium hydroxide by phenylpropyl alcohol building emulsion to 45 DEG C
Value, makes the pH value 8 of pure phenylpropyl alcohol building emulsion.
Wherein, composite emulsifier includes lauryl sodium sulfate, Value 3608, ten alcohol polyoxy second of isomery
Alkene ether, allyloxy hydroxypropyl azochlorosulfonate acid sodium: Value 3608: the weight proportion of heterogeneous ten alcohol polyoxyethylene ether is
4:1.3:1, and lauryl sodium sulfate, Value 3608, heterogeneous ten alcohol polyoxyethylene ether are mixed by stirring
It closes uniformly, composite emulsifier can be obtained.
Wherein, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is prepared using following methods: being added in mixing kettle
1/10 water is added in mixing kettle then by the way of sprinkling for MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, stirring
Remaining water is added in mixing kettle later by 2min, is uniformly mixed, it is molten to obtain MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride
Liquid.
Embodiment 2
A kind of pure phenylpropyl alcohol building emulsion, raw material proportioning are shown in Table 1, table 2；
(1) in mixing kettle, water, allyloxy hydroxypropyl azochlorosulfonate acid sodium reaction emulsifier, sodium bicarbonate is uniformly mixed, kettle is obtained
Bottom solution, it is spare；
(2) in another mixing kettle, by water, composite emulsifier, n-butyl acrylate, styrene, acrylamide, acrylic acid
It is uniformly mixed, the weight proportion of n-butyl acrylate and styrene is 1:1 at this time, obtains mixed monomer solution, spare；
(3) bottom solution is added in a kettle, and under conditions of temperature is 83 DEG C, adds in the bottom solution into reaction kettle
Enter just initiator, it is 18.33% ammonium persulfate solution that first initiator, which selects mass fraction, and just reaction kettle is being added in initiator
Preceding 20min, which is prepared, to be completed, and controls temperature at 86 DEG C, then by the way of being added dropwise, it is single that mixing is added dropwise into reaction kettle respectively
Liquid solution and reaction initiator, the ammonium persulfate solution that reaction initiator selection mass fraction is 4.14%, and reaction initiator
20min before reaction kettle is added, which is prepared, to be completed, and mixed monomer solution and reaction initiator are added dropwise in 3.5h, later
The MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution that mass fraction is 1.78%, methacryloxypropyl are added into reaction kettle
2min of the ethyl-trimethyl salmiac solution before reaction kettle is added, which is prepared, to be completed, insulation reaction 1.5h；
(4) by most 70 DEG C of the greenhouse cooling in reaction kettle, oxidant is added, it is 10% tert-butyl that oxidant, which selects mass fraction,
Reducing agent is added in hydrogenperoxide steam generator, insulation reaction 7min, and it is 3% rongalite solution that reducing agent, which selects mass fraction, and heat preservation is anti-
20min is answered, polyoxyethylene polyoxy Propanolamine ether defoaming agent, Brassicol are added later, is uniformly mixed, obtains pure
Then greenhouse cooling in reaction kettle is used mass fraction to adjust its pH for 5% ammonium hydroxide by phenylpropyl alcohol building emulsion to 45 DEG C
Value, makes the pH value 8.5 of pure phenylpropyl alcohol building emulsion.
Wherein, composite emulsifier includes lauryl sodium sulfate, Value 3608, ten alcohol polyoxy second of isomery
Alkene ether, allyloxy hydroxypropyl azochlorosulfonate acid sodium: Value 3608: the weight proportion of heterogeneous ten alcohol polyoxyethylene ether is
4:1.3:1, and lauryl sodium sulfate, Value 3608, heterogeneous ten alcohol polyoxyethylene ether are mixed by stirring
It closes uniformly, composite emulsifier can be obtained.
Wherein, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is prepared using following methods: being added in mixing kettle
1/10 water is added in mixing kettle then by the way of sprinkling for MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, stirring
Remaining water is added in mixing kettle later by 2min, is uniformly mixed, it is molten to obtain MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride
Liquid.
Embodiment 3
A kind of pure phenylpropyl alcohol building emulsion, raw material proportioning are shown in Table 1, table 2；
(1) in mixing kettle, water, allyloxy hydroxypropyl azochlorosulfonate acid sodium reaction emulsifier, sodium bicarbonate is uniformly mixed, kettle is obtained
Bottom solution, it is spare；
(2) in another mixing kettle, by water, composite emulsifier, n-butyl acrylate, styrene, acrylamide, acrylic acid
It is uniformly mixed, the weight proportion of n-butyl acrylate and styrene is 1:1 at this time, obtains mixed monomer solution, spare；
(3) bottom solution is added in a kettle, and under conditions of temperature is 83 DEG C, adds in the bottom solution into reaction kettle
Enter just initiator, it is 18.33% ammonium persulfate solution that first initiator, which selects mass fraction, and just reaction kettle is being added in initiator
Preceding 10min, which is prepared, to be completed, and controls temperature at 86 DEG C, then by the way of being added dropwise, it is single that mixing is added dropwise into reaction kettle respectively
Liquid solution and reaction initiator, the ammonium persulfate solution that reaction initiator selection mass fraction is 4.14%, and reaction initiator
10min before reaction kettle is added, which is prepared, to be completed, and mixed monomer solution and reaction initiator are added dropwise in 3h, backward
The MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution that mass fraction is 1.78%, methacryloxypropyl second are added in reaction kettle
3min of the base trimethyl ammonia chloride ammonium salt solution before reaction kettle is added, which is prepared, to be completed, insulation reaction 2h；
(4) by most 70 DEG C of the greenhouse cooling in reaction kettle, oxidant is added, it is 10% tert-butyl that oxidant, which selects mass fraction,
Reducing agent is added in hydrogenperoxide steam generator, insulation reaction 6min, and it is 3% rongalite solution that reducing agent, which selects mass fraction, and heat preservation is anti-
35min is answered, polyoxyethylene polyoxy Propanolamine ether defoaming agent, Brassicol are added later, is uniformly mixed, obtains pure
Then greenhouse cooling in reaction kettle is used mass fraction to adjust its pH for 5% ammonium hydroxide by phenylpropyl alcohol building emulsion to 45 DEG C
Value, makes the pH value 8 of pure phenylpropyl alcohol building emulsion.
Wherein, composite emulsifier includes lauryl sodium sulfate, Value 3608, ten alcohol polyoxy second of isomery
Alkene ether, allyloxy hydroxypropyl azochlorosulfonate acid sodium: Value 3608: the weight proportion of heterogeneous ten alcohol polyoxyethylene ether is
4:1.3:1, and lauryl sodium sulfate, Value 3608, heterogeneous ten alcohol polyoxyethylene ether are mixed by stirring
It closes uniformly, composite emulsifier can be obtained.
Wherein, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is prepared using following methods: being added in mixing kettle
1/10 water is added in mixing kettle then by the way of sprinkling for MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, stirring
Remaining water is added in mixing kettle later by 2min, is uniformly mixed, it is molten to obtain MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride
Liquid.
Embodiment 4
A kind of pure phenylpropyl alcohol building emulsion, raw material proportioning are shown in Table 1, table 2；
(1) in mixing kettle, water, allyloxy hydroxypropyl azochlorosulfonate acid sodium reaction emulsifier, sodium bicarbonate is uniformly mixed, kettle is obtained
Bottom solution, it is spare；
(2) in another mixing kettle, by water, composite emulsifier, n-butyl acrylate, styrene, acrylamide, acrylic acid
It is uniformly mixed, the weight proportion of n-butyl acrylate and styrene is 1:1 at this time, obtains mixed monomer solution, spare；
(3) bottom solution is added in a kettle, and under conditions of temperature is 83 DEG C, adds in the bottom solution into reaction kettle
Enter just initiator, it is 18.33% ammonium persulfate solution that first initiator, which selects mass fraction, and just reaction kettle is being added in initiator
Preceding 5min, which is prepared, to be completed, and controls temperature at 86 DEG C, then by the way of being added dropwise, mix monomer is added dropwise into reaction kettle respectively
Solution and reaction initiator, it is 4.14% ammonium persulfate solution that reaction initiator, which selects mass fraction, and reaction initiator exists
5min before reaction kettle is added, which is prepared, to be completed, and mixed monomer solution and reaction initiator are added dropwise in 2.5h, backward
The MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution that mass fraction is 1.78%, methacryloxypropyl second are added in reaction kettle
3min of the base trimethyl ammonia chloride ammonium salt solution before reaction kettle is added, which is prepared, to be completed, insulation reaction 2.5h；
(4) by most 70 DEG C of the greenhouse cooling in reaction kettle, oxidant is added, it is 10% tert-butyl that oxidant, which selects mass fraction,
Reducing agent is added in hydrogenperoxide steam generator, insulation reaction 8min, and it is 3% rongalite solution that reducing agent, which selects mass fraction, and heat preservation is anti-
10min is answered, polyoxyethylene polyoxy Propanolamine ether defoaming agent, Brassicol are added later, is uniformly mixed, obtains pure
Then greenhouse cooling in reaction kettle is used mass fraction to adjust its pH for 5% ammonium hydroxide by phenylpropyl alcohol building emulsion to 45 DEG C
Value, makes the pH value 9 of pure phenylpropyl alcohol building emulsion.
Wherein, composite emulsifier includes lauryl sodium sulfate, Value 3608, ten alcohol polyoxy second of isomery
Alkene ether, allyloxy hydroxypropyl azochlorosulfonate acid sodium: Value 3608: the weight proportion of heterogeneous ten alcohol polyoxyethylene ether is
4:1.3:1, and lauryl sodium sulfate, Value 3608, heterogeneous ten alcohol polyoxyethylene ether are mixed by stirring
It closes uniformly, composite emulsifier can be obtained.
Wherein, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is prepared using following methods: being added in mixing kettle
1/10 water is added in mixing kettle then by the way of sprinkling for MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, stirring
Remaining water is added in mixing kettle later by 2min, is uniformly mixed, it is molten to obtain MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride
Liquid.
Embodiment 5
A kind of pure phenylpropyl alcohol building emulsion, raw material proportioning are shown in Table 1, table 2；
(1) in mixing kettle, water, allyloxy hydroxypropyl azochlorosulfonate acid sodium reaction emulsifier, sodium bicarbonate is uniformly mixed, kettle is obtained
Bottom solution, it is spare；
(2) in another mixing kettle, by water, composite emulsifier, n-butyl acrylate, styrene, acrylamide, acrylic acid
It is uniformly mixed, the weight proportion of n-butyl acrylate and styrene is 1:1 at this time, obtains mixed monomer solution, spare；
(3) bottom solution is added in a kettle, and under conditions of temperature is 83 DEG C, adds in the bottom solution into reaction kettle
Enter just initiator, it is 18.33% ammonium persulfate solution that first initiator, which selects mass fraction, and just reaction kettle is being added in initiator
Preceding 10min, which is prepared, to be completed, and controls temperature at 86 DEG C, then by the way of being added dropwise, it is single that mixing is added dropwise into reaction kettle respectively
Liquid solution and reaction initiator, the ammonium persulfate solution that reaction initiator selection mass fraction is 4.14%, and reaction initiator
10min before reaction kettle is added, which is prepared, to be completed, and mixed monomer solution and reaction initiator are added dropwise in 4h, backward
The MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution that mass fraction is 1.78%, methacryloxypropyl second are added in reaction kettle
3min of the base trimethyl ammonia chloride ammonium salt solution before reaction kettle is added, which is prepared, to be completed, insulation reaction 1h；
(4) by most 70 DEG C of the greenhouse cooling in reaction kettle, oxidant is added, it is 10% tert-butyl that oxidant, which selects mass fraction,
Reducing agent is added in hydrogenperoxide steam generator, insulation reaction 4min, and it is 3% rongalite solution that reducing agent, which selects mass fraction, and heat preservation is anti-
60min is answered, polyoxyethylene polyoxy Propanolamine ether defoaming agent, Brassicol are added later, is uniformly mixed, obtains pure
Then greenhouse cooling in reaction kettle is used mass fraction to adjust its pH for 5% ammonium hydroxide by phenylpropyl alcohol building emulsion to 45 DEG C
Value, makes the pH value 7.5 of pure phenylpropyl alcohol building emulsion.
Wherein, composite emulsifier includes lauryl sodium sulfate, Value 3608, ten alcohol polyoxy second of isomery
Alkene ether, allyloxy hydroxypropyl azochlorosulfonate acid sodium: Value 3608: the weight proportion of heterogeneous ten alcohol polyoxyethylene ether is
4:1.3:1, and lauryl sodium sulfate, Value 3608, heterogeneous ten alcohol polyoxyethylene ether are mixed by stirring
It closes uniformly, composite emulsifier can be obtained.
Wherein, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is prepared using following methods: being added in mixing kettle
1/10 water is added in mixing kettle then by the way of sprinkling for MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, stirring
Remaining water is added in mixing kettle later by 2min, is uniformly mixed, it is molten to obtain MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride
Liquid.
Comparative example 1
The difference of comparative example 1 and embodiment 3 is, is not added with methylacryoyloxyethyl in the raw material of pure phenylpropyl alcohol building emulsion
Trimethyl ammonia chloride ammonium salt solution.
Comparative example 2
The difference of comparative example 2 and embodiment 3 is, Value 3608, isomery ten are not added in composite emulsifier
Alcohol polyoxyethylene ether.
Comparative example 3
The difference of comparative example 3 and embodiment 3 is, reaction emulsifier is replaced with composite emulsifier.
Comparative example 4
The difference of comparative example 4 and embodiment 3 is, composite emulsifier is replaced with reaction emulsifier.
Comparative example 5
The difference of comparative example 5 and embodiment 3 is that the mass fraction of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is
1.9%.
Comparative example 6
The difference of comparative example 6 and embodiment 3 is that the mass fraction of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is
1.6%.
Comparative example 7
The difference of comparative example 7 and embodiment 3 is that MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is matched using preceding 6min
System is completed.
Comparative example 8
The difference of comparative example 8 and embodiment 3 is that first initiator, reaction initiator are preparing completion using preceding 50min.
The pure phenylpropyl alcohol building emulsion obtained respectively to embodiment 1-5 and comparative example 1-8, carries out following performance detections, inspection
The results are shown in Table 3 for survey.
Wherein, in Ca2+In Detection of Stability, calcium chloride solution: the weight proportion of lotion is 1:4, and calcium chloride solution
Mass fraction is 5%.
3 testing result of table
From table 3 it is observed that pure phenylpropyl alcohol building emulsion of the invention, solid content with higher, glass transition temperature, admittedly contain
Amount up to 49%, glass transition temperature is up to 25 DEG C, but also has lower viscosity, partial size, the minimum 520Pa.s of viscosity
×10-3, the minimum 0.094um of partial size, and film-forming temperature is 19 DEG C, while in 5% calcium chloride solution: the weight proportion of lotion
It when for 1:4, is stabilized, is not demulsified, therefore also have the advantages that storage stability, and be suitable for matt latex paint, semi-gloss cream
In shellac varnish.
By comparative example 3 and comparative example 1, comparative example 5-6, it can thus be seen that metering system is added in the feed
Acyloxyethyl trimethyl ammonia chloride ammonium salt solution, and the mass fraction of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution is 1.78%
When, pure phenylpropyl alcohol building emulsion surface goes out good partial size, while mixing is added in MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride
In monomer solution, and polymerization reaction occurs between the raw material of mixed monomer solution, not only increases its antibiotic property, and make cream
The electric double layer of liquid ion is more stable, to improve the uniformity of its partial size, and reduces partial size, and also improves its calcium
The stability of ion.
By comparative example 3 and comparative example 2-4, it can thus be seen that by composite emulsifier and reaction emulsifier it
Between synergistic effect, composite emulsifier improves water, n-butyl acrylate, styrene, acrylamide, mixes between acrylic acid
Uniformity, and it is uniformly dispersed in organic matter in water, stable solution is formed, subsequent generation Raolical polymerizable is convenient for,
Reaction emulsifier is added in the solution of bottom simultaneously, when bottom solution is added in mixed monomer solution, enables mixed monomer solution
It is enough to be quickly uniformly mixed with bottom solution, and by the radical polymerization in the solution of bottom, to accelerate free radical
Polymerization reaction, since bottom solution is different with raw material difference, the difference of blending constituent, the ratio of mixed monomer solution, purpose
It is not identical, so that composite emulsifier is different with the formula of reaction emulsifier, so that it is good to have pure phenylpropyl alcohol building emulsion
Solid content well, partial size, viscosity, stability.
By comparative example 3 and comparative example 7-8, it can thus be seen that just initiator is formed centainly in the solution of bottom
The free radical of amount, reaction initiator makes to maintain metastable number of free radical in Raolical polymerizable system, by just drawing
The synergistic effect between agent and reaction initiator is sent out, the efficiency of Raolical polymerizable is accelerated, first initiator, reaction are caused
The preparation time of agent is defined, and the preparation time of first initiator, reaction initiator is avoided to reduce oneself generated in it too early
By base, to improve the performance of pure phenylpropyl alcohol building emulsion.
Claims (10)
1. a kind of pure phenylpropyl alcohol building emulsion, it is characterised in that: according to parts by weight, raw material includes 700-1000 parts of water, answers
With 6.5-10 parts of emulsifier, 855-1040 parts of n-butyl acrylate, 855-1040 parts of styrene, 34-50 parts of acrylamide, propylene
22-34 parts sour, solution 846-1122 parts of bottom, initiator 28-42 parts first, 120-180 parts of reaction initiator, methacryloxypropyl
93-134 parts of ethyl-trimethyl salmiac solution, 13.2-19.8 parts of oxidant, 41-61 parts of reducing agent, 1.5-2.5 parts of defoaming agent,
1.5-2.5 parts of fungicide, the bottom solution includes 800-1200 parts of water, 7.8-11 parts of reaction emulsifier, sodium bicarbonate 1-1.4
Part, the weight proportion of the n-butyl acrylate and styrene is 1:1, and the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride is molten
The mass fraction of liquid is 1.78%.
2. a kind of pure phenylpropyl alcohol building emulsion according to claim 1, it is characterised in that: its raw material includes water 750-900
Part, 7.5-9.2 parts of composite emulsifier, 900-968 parts of n-butyl acrylate, 900-968 parts of styrene, 39-46 parts of acrylamide,
25-30 parts of acrylic acid, solution 923-1084 parts of bottom, initiator 32-39 parts first, 135-165 parts of reaction initiator, metering system
108-134 parts of acyloxyethyl trimethyl ammonia chloride ammonium salt solution, 14.8-18.1 parts of oxidant, 46.3-51.5 parts of reducing agent, defoaming agent
1.8-2.2 parts, 1.8-2.2 parts of fungicide, the bottom solution include 900-1100 parts of water, 8.5-10.5 parts of reaction emulsifier,
1.1-1.3 parts of sodium bicarbonate.
3. a kind of pure phenylpropyl alcohol building emulsion according to claim 1, it is characterised in that: the just initiator is quality point
The ammonium persulfate solution that number is 18.33%, the reaction initiator are the ammonium persulfate solutions that mass fraction is 4.14%.
4. a kind of pure phenylpropyl alcohol building emulsion according to claim 1, it is characterised in that: the pure phenylpropyl alcohol building emulsion
PH value control between 7.5-9.
5. a kind of pure phenylpropyl alcohol building emulsion according to claim 1, it is characterised in that: the composite emulsifier includes ten
Sodium dialkyl sulfate, Value 3608, heterogeneous ten alcohol polyoxyethylene ether, the allyloxy hydroxypropyl sulfonic acid
Sodium: Value 3608: the weight proportion of heterogeneous ten alcohol polyoxyethylene ether is 4:1.3:1.
6. a kind of pure phenylpropyl alcohol building emulsion according to claim 1, it is characterised in that: the reaction emulsifier is allyl
Oxygroup hydroxypropyl azochlorosulfonate acid sodium.
7. a kind of pure phenylpropyl alcohol building emulsion according to claim 1, it is characterised in that: the oxidant is mass fraction
For 10% tert-butyl hydroperoxide solution, the reducing agent is that mass fraction is 3% rongalite solution.
It prepares a kind of method of pure phenylpropyl alcohol building emulsion, feature described in any one of claim 1-7 8. a kind of and exists
In: include the following steps:
(1) water, reaction emulsifier, sodium bicarbonate are uniformly mixed, obtain bottom solution, it is spare；
(2) water, composite emulsifier, n-butyl acrylate, styrene, acrylamide, acrylic acid are uniformly mixed, it is single obtains mixing
Liquid solution, it is spare；
(3) under conditions of temperature is 83 DEG C, just initiator is added into bottom solution, then by the way of being added dropwise, respectively
Mixed monomer solution and reaction initiator is added dropwise, and controls temperature and is added dropwise at 86 DEG C, and in 2-4h, methyl is added later
Acrylyl oxy-ethyl-trimethyl salmiac solution, insulation reaction 1-3h；
(4) cool down most 70 DEG C, addition oxidant, insulation reaction 4-8min, addition reducing agent, insulation reaction 10-60min, it
Defoaming agent, fungicide are added afterwards, is uniformly mixed, obtains pure phenylpropyl alcohol building emulsion.
9. a kind of method for preparing pure phenylpropyl alcohol building emulsion according to claim 8, it is characterised in that: the pure benzene
Third building emulsion adjusts pH value using ammonium hydroxide, and the mass fraction of the ammonium hydroxide is 5%.
10. a kind of method for preparing pure phenylpropyl alcohol building emulsion according to claim 8, it is characterised in that: described just to draw
It sends out agent, reaction initiator to complete using preparation in preceding 30min, the MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride solution
It is completed using preparation in preceding 3min.
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| CN111234082A (en) * | 2020-03-12 | 2020-06-05 | 广东巴德富新材料有限公司 | Amphoteric emulsion for permeation-sealed primer and preparation method thereof |
| CN113265182A (en) * | 2021-06-23 | 2021-08-17 | 广东金万联防水材料有限公司 | Preparation method of novel waterproof coating |
| CN113549171A (en) * | 2021-07-22 | 2021-10-26 | 武汉工程大学 | Diatomite modified styrene-acrylic emulsion for humidity-controlling coating and preparation method and application thereof |
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