CN103554334B - The monomer modified acrylate of internal plasticization/inorganic nano combined emulsion and preparation method thereof - Google Patents
The monomer modified acrylate of internal plasticization/inorganic nano combined emulsion and preparation method thereof Download PDFInfo
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Abstract
The invention discloses the monomer modified acrylate of a kind of internal plasticization/inorganic nano combined emulsion and preparation method thereof.Its raw material is composed of the following components according to weight percent: acrylate monomer: 30 ~ 60%, internal plasticization monomer: 1 ~ 10%, inorganic nano material: 1 ~ 10%, initiator: 0.1 ~ 1%, emulsifying agent: 1 ~ 10%, buffer reagent: 0.01 ~ 1%, lauryl mercaptan: 0.01 ~ 1%, surplus is deionized water.Internal plasticization monomer directly pre-emulsification together with acrylate monomer in preparation method, inorganic nano material is disposable directly to add, and production process required equipment is simple, easy to operate, cost is lower, security is high.The present invention adopts internal plasticization monomer and inorganic nano material comprehensively modifying acrylic ester emulsion, and not only have high strength after film forming, toughness also increases substantially, and glossiness and resistance toheat also increase substantially, and has widened the application category of emulsion.
Description
Technical field
The present invention relates to modified acrylate emulsion, refer to the monomer modified acrylate of a kind of internal plasticization/inorganic nano combined emulsion and preparation method thereof particularly.
Background technology
Acrylic ester emulsion with water as medium, production safety, environmental pollution is little, overcomes the shortcoming that solvent based polymer is fatal, meets the requirement of people to the Chemicals feature of environmental protection; Simultaneously acrylate monomer abundant raw material source, with low cost, production equipment and process is simple, easy to operate, handiness is large; And this class emulsion property is excellent, have good stability (storage, freeze thawing, machinery etc.), film clarity is high, glossiness good, ageing-resistant, water tolerance and acid-proof.These advantages impart acrylic ester emulsion purposes widely, can be used for water-borne coatings, writing material, tackiness agent and functional membrane, and the consumption in the industry such as building, medicine, automobile and papermaking grows with each passing day.
Along with people are more and more higher to environmental requirement, the consumption of water-and acrylate emulsion is much larger than the consumption of solvent-type acrylic fat.But acrylic ester emulsion also also exists the shortcoming that low temperature becomes fragile, high temperature becomes sticky, affect toughness and the intensity of film, limit to a certain extent its application, and the toughness of latex film and intensity conflicting.Common method of modifying is all reduce intensity to improve toughness, or reduction toughness improves intensity.
Although the monomer modified acrylate of existing internal plasticization can improve the toughness of latex film, but conventional internal plasticization monomer is as made the side base on macromolecular chain increase after the internal plasticization monomers such as dibutyl maleinate, dibutyl itaconate, dibutyl fumarate and acrylic ester emulsion copolymerization, molecular chain irregularity degree increases, also make the distance between polymer molecular chain increase simultaneously, Intermolecular Forces weakens, therefore tensile strength can be made to reduce, and thermotolerance is deteriorated.
In addition, along with the continuous innovation of the technology such as aerospace, automobile, military project, petrochemical complex, metallurgy, electronic apparatus, building, equipment work temperature improves constantly, and the heat insulating and corrosion erosion resisting coating of high temperature service is very important, and high-temperature resistant coating consumption increases day by day.As the device external such as industrial chimney, high temperature steam pipeline, mould, interchanger, High Temperature Furnaces Heating Apparatus, high temperature desulfurizing equipment, petrochemical industry cracking apparatus, engine parts, vapor pipe all need high-temperature resistant coating.Therefore, the thermotolerance improving acrylic ester aquosity coating, at the equipment of hot environment work and important, also can improve the thermostability of coating under extreme weather.
The glossiness of coating and ink is mainly produced by emulsion conjunctiva, and the outward appearance of glossiness on coating or ink goods brings very large impact, and glossiness is high, then bright in colour, seems more spiritual, caters to needing of people at heart; Low in glossiness, then color and luster is dim, outmoded to people's one, and depressed sensation, reduces the effect of publicity of product greatly.At present, water color ink and the inadequate shortcoming of water-borne coatings ubiquity glossiness, except for the outer the reason such as light source, base material, the composition of itself of ink and coating and character can play decisive role to glossiness.
Summary of the invention
Object of the present invention is exactly to overcome the deficiency existing for prior art, provides the monomer modified acrylate of a kind of internal plasticization/inorganic nano combined emulsion and preparation method thereof.
The monomer modified acrylate of internal plasticization provided by the present invention/inorganic nano combined emulsion, its raw material is composed of the following components according to weight percent:
Preferably, the raw material of the monomer modified acrylate of internal plasticization/inorganic nano combined emulsion is composed of the following components according to weight percent:
Wherein, described internal plasticization monomer is any one or multiple composite use in dibutyl maleinate, dibutyl itaconate, dibutyl fumarate, monobutyl itaconate, butyl maleate, dioctyl maleate.Described internal plasticization monomer is preferably dibutyl itaconate or monobutyl itaconate.
Described inorganic nano material is any one or multiple composite use in calcium carbonate, aluminum oxide, silicon-dioxide, titanium dioxide, zinc oxide, polynite.Described inorganic nano material is preferably aluminum oxide, silicon-dioxide, titanium dioxide or zinc oxide.
In the present invention, emulsifying agent used is any one or two kinds of composite uses in allyloxy sulfated alkyl ether, polyoxyethylene alkyl ether sulfate salt, sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, alkylphenol polyoxyethylene.
In the present invention, initiator used is any one or two kinds of composite uses in ammonium persulphate, Potassium Persulphate, Potassium hydrogen sulfite, Potassium Thiosulphate.
In the present invention, described buffer reagent used is any one in bicarbonate of ammonia, sodium bicarbonate, Calcium hydrogen carbonate, ammoniacal liquor.
The preparation method of the monomer modified acrylate of above-mentioned internal plasticization/inorganic nano combined emulsion, comprises the following steps:
1. according to weight proportion by emulsifying agent, lauryl mercaptan, acrylate monomer and internal plasticization monomer, be added in the deionized water accounting for deionized water gross weight 20 ~ 40% used, stirring at normal temperature mixes, and is prepared into pre-emulsion;
2. initiator and buffer reagent are added in the deionized water accounting for deionized water gross weight 20 ~ 40% used, stirring at normal temperature mixes, and is prepared into initiation solution;
3. inorganic nano material is added in the deionized water accounting for deionized water gross weight 20 ~ 40% used, be warming up to 70 ~ 85, DEG C add 20 ~ 40% of the initiation solution gross weight that 2. step is prepared, by the time temperature is raised to 70 ~ 85 again, DEG C adds 3 ~ 15% of the pre-emulsion gross weight that 1. step is prepared;
4. blue light is produced after 3 ~ 10 minutes, temperature of reaction controls 70 ~ 85, DEG C to drip initiation solution that 2. remaining step prepared and the pre-emulsion that 1. remaining step is prepared, time for adding controlled at 2 ~ 4.5 hours, and made initiation solution add complete in 3-10 minute after pre-emulsion dropwises simultaneously;
5. temperature is risen to 85 ~ 90 DEG C of slakings 1 ~ 2 hour, be naturally down to room temperature, filter discharging, obtain the monomer modified acrylate of internal plasticization/inorganic nano combined emulsion.
For the feature of acrylic ester emulsion hot sticky cold crisp, the present invention adopts internal plasticization monomer and inorganic nano material comprehensively modifying acrylic ester emulsion.Internal plasticization monomer can give plasticity and the elasticity of acrylic ester emulsion excellence, and compared with conventional plasticizers, internal plasticization monomer can be avoided external plasticizer to cause because of the impact of the factors such as migration, precipitation, volatilization and mould goods problem of aging, is permanent plasticization effect.And adding of inorganic nano material can obtain Organic-inorganic composite emulsion, can significantly improve latex film strength, toughness and thermotolerance, realize the complementation between different components performance.
The present invention is main monomer with acrylate monomer, and the soft or hard degree of relative content to latex film between monomer has a significant impact, and can need to regulate the soft or hard degree of film according to practical application.
Beneficial effect of the present invention is: adopt the modified acrylate composite emulsion of the present invention, not only have high strength after film forming, toughness also increases substantially, and solves that acrylic ester emulsion low temperature becomes fragile, high temperature becomes sticky and affects the problem being coated with film toughness and intensity.
The acrylate composite emulsion that the present invention is modified, high comprehensive performance, film-forming properties, solvent resistance, the shock resistance of the good dilution of existing conventional acrylates emulsion, freeze thawing, mechanical stability and excellence, can increase substantially again the toughness of latex film while ensureing latex film intensity.
The present invention is by internal plasticization monomer and inorganic nano material modified, and the glossiness of latex film improves greatly, and also monomer modified than the independent internal plasticization latex film of resistance toheat increases substantially, and has widened the application category of emulsion.The modified acrylate composite emulsion of the present invention not only can be used for water-borne coatings, writing material, tackiness agent and functional membrane etc., can also be used on high temperature service as high-temperature resistant coating.
And internal plasticization monomer is pre-emulsification together with acrylate monomer directly, and inorganic nano material is disposable directly to add, and production process required equipment is simple, easy to operate, cost is lower, security is high.
Embodiment
In order to explain the present invention better, below in conjunction with specific embodiment, the present invention is described in further detail, but they do not form restriction to the present invention.
In the present invention, acrylate monomer used is conventional several, such as, methyl methacrylate, methyl acrylate, ethyl propenoate, β-dimethyl-aminoethylmethacrylate, n-butyl acrylate, n-BMA, isobutyl acrylate, glycidyl methacrylate, methacrylic acid-2-ethylhexyl, methacrylic acid-2-hydroxy propyl ester or lauryl acrylate.
Embodiment 1
1. in the reactor with agitator, condenser, add 46.8g deionized water, 3.5g sodium lauryl sulphate, 0.06g lauryl mercaptan, 145g acrylate main monomer and 5.3g dibutyl maleinate, stirring at normal temperature mixes, and is prepared into pre-emulsion;
2. 0.6g Potassium Persulphate and 0.09g sodium bicarbonate are dissolved in 46.8g deionized water, stirring at normal temperature mixes, and is prepared into initiation solution;
3. in the reactor with agitator, condenser, constant flow pump feeding device, 2.4g nano-calcium carbonate and 62.4g deionized water is added, be warming up to 78, DEG C in reactor, add 30% of the initiation solution gross weight that 2. step is prepared, by the time temperature is raised to 78 again, DEG C in reactor, adds 3% of the pre-emulsion gross weight that 1. step is prepared;
4. within 3 ~ 10 minutes, in post-reactor, blue light is produced, temperature of reaction controls 78 ~ 80, DEG C in reactor, drip initiation solution that 2. remaining step prepared and the pre-emulsion that 1. remaining step is prepared by constant flow pump simultaneously, time for adding controlled at 2 ~ 4.5 hours, and made initiation solution add complete in 3 ~ 10 minutes after pre-emulsion dropwises;
5. temperature is risen to 90 DEG C of slakings 1 ~ 2 hour, be naturally down to room temperature, filter discharging, can obtain band blue light, solid content is 49.07%, and transformation efficiency is the monomer modified acrylate of the internal plasticization/inorganic nano combined emulsion of 98.14%.
Embodiment 2
1. in the reactor with agitator, condenser, add 48.3g deionized water, 3.5g Sodium dodecylbenzene sulfonate, 0.06g lauryl mercaptan, 145g acrylate main monomer and 5.3g butyl maleate, stirring at normal temperature mixes, and is prepared into pre-emulsion;
2. 0.6g ammonium persulphate and 0.09g bicarbonate of ammonia are dissolved in 48.3g deionized water, stirring at normal temperature mixes, and is prepared into initiation solution;
3. in the reactor with agitator, condenser, constant flow pump feeding device, 7.2g nano imvite and 64.4g deionized water is added, be warming up to 78, DEG C in reactor, add 35% of the initiation solution gross weight that 2. step is prepared, by the time temperature is raised to 78 again, DEG C in reactor, adds 8% of the pre-emulsion gross weight that 1. step is prepared;
4. within 3 ~ 10 minutes, in post-reactor, blue light is produced, temperature of reaction controls 78 ~ 80, DEG C in reactor, drip initiation solution that 2. remaining step prepared and the pre-emulsion that 1. remaining step is prepared by constant flow pump simultaneously, time for adding controlled at 2 ~ 4.5 hours, and made initiation solution add complete in 3 ~ 10 minutes after pre-emulsion dropwises;
5. temperature is risen to 90 DEG C of slakings 1 ~ 2 hour, be naturally down to room temperature, filter discharging, namely obtain being with the monomer modified acrylate of internal plasticization/inorganic nano combined emulsion that blue light, solid content are 49.23%, transformation efficiency is 98.46%.
Embodiment 3
1. in the reactor with agitator, condenser, add 49.8g deionized water, 3.5g alkylphenol polyoxyethylene, 0.06g lauryl mercaptan, 145g acrylate main monomer and 5.3g dibutyl fumarate, stirring at normal temperature mixes, and is prepared into pre-emulsion;
2. 0.6g Potassium Thiosulphate and 0.09g ammoniacal liquor are dissolved in 49.8g deionized water, stirring at normal temperature mixes, and is prepared into initiation solution;
3. in the reactor with agitator, condenser, constant flow pump feeding device, 12.08g nano aluminium oxide and 66.4g deionized water is added, be warming up to 78, DEG C in reactor, add 40% of the initiation solution gross weight that 2. step is prepared, by the time temperature is raised to 78 again, DEG C in reactor, adds 12% of the pre-emulsion gross weight that 1. step is prepared;
4. within 3 ~ 10 minutes, in post-reactor, blue light is produced, temperature of reaction controls at 78 ~ 80 DEG C, in reactor, drip 2. remaining step prepared initiation solution and the pre-emulsion that 1. remaining step is prepared by constant flow pump simultaneously, time for adding controlled at 2 ~ 4.5 hours, and made initiation solution add complete in 3 ~ 10 minutes after pre-emulsion dropwises;
5. temperature is risen to 90 slaking 1 ~ 2 hour, be naturally down to room temperature, filter discharging, namely obtain being with the monomer modified acrylate of internal plasticization/inorganic nano combined emulsion that blue light, solid content are 48.72%, transformation efficiency is 97.44%.
Embodiment 4
1. in the reactor with agitator, condenser, add 49.8g deionized water, 3.5g sodium lauryl sulphate, 0.06g lauryl mercaptan, 145g acrylate main monomer and 5.3g monobutyl itaconate, stirring at normal temperature mixes, and is prepared into pre-emulsion;
2. 0.6g Potassium Persulphate-Potassium hydrogen sulfite and 0.09g Calcium hydrogen carbonate are dissolved in 49.8g deionized water, stirring at normal temperature mixes, and is prepared into initiation solution;
3. in the reactor with agitator, condenser, constant flow pump feeding device, 12.08g nano silicon and 66.4g deionized water is added, be warming up to 78, DEG C in reactor, add 20% of the initiation solution gross weight that 2. step is prepared, by the time temperature is raised to 78 again, DEG C in reactor, adds 10% of the pre-emulsion gross weight that 1. step is prepared;
4. within 3 ~ 10 minutes, in post-reactor, blue light is produced, temperature of reaction controls at 78 ~ 80 DEG C, in reactor, drip 2. remaining step prepared initiation solution and the pre-emulsion that 1. remaining step is prepared by constant flow pump simultaneously, time for adding controlled at 2 ~ 4.5 hours, and made initiation solution add complete in 3 ~ 10 minutes after pre-emulsion dropwises;
5. temperature is risen to 90 slaking 1 ~ 2 hour, be naturally down to room temperature, filter discharging, namely obtain being with the monomer modified acrylate of internal plasticization/inorganic nano combined emulsion that blue light, solid content are 49.42%, transformation efficiency is 98.84%.
Embodiment 5
1. in the reactor with agitator, condenser, add 49.8g deionized water, 3.5g sodium lauryl sulphate, 0.06g lauryl mercaptan, 145g acrylate main monomer and 5.3g dibutyl itaconate, stirring at normal temperature mixes, and is prepared into pre-emulsion;
2. 0.6g Potassium Persulphate-Potassium hydrogen sulfite and 0.09g Calcium hydrogen carbonate are dissolved in 49.8g deionized water, stirring at normal temperature mixes, and is prepared into initiation solution;
3. in the reactor with agitator, condenser, constant flow pump feeding device, 12.08g nano titanium oxide and 66.4g deionized water is added, be warming up to 78, DEG C in reactor, add 20% of the initiation solution gross weight that 2. step is prepared, by the time temperature is raised to 78 again, DEG C in reactor, adds 10% of the pre-emulsion gross weight that 1. step is prepared;
4. within 3 ~ 10 minutes, in post-reactor, blue light is produced, temperature of reaction controls at 78 ~ 80 DEG C, in reactor, drip 2. remaining step prepared initiation solution and the pre-emulsion that 1. remaining step is prepared by constant flow pump simultaneously, time for adding controlled at 2 ~ 4.5 hours, and made initiation solution add complete in 3 ~ 10 minutes after pre-emulsion dropwises;
5. temperature is risen to 90 slaking 1 ~ 2 hour, be naturally down to room temperature, filter discharging, namely obtain being with the monomer modified acrylate of internal plasticization/inorganic nano combined emulsion that blue light, solid content are 49.51%, transformation efficiency is 99.02%.
Comparative example 1
1. in the reactor with agitator, condenser, add 46.2g deionized water, 3.5g sodium lauryl sulphate, 0.06g lauryl mercaptan and 150g methyl methacrylate, stirring at normal temperature mixes, and is prepared into pre-emulsion;
2. 0.6g Potassium Persulphate and 0.09g sodium bicarbonate are dissolved in 46.2g deionized water, stirring at normal temperature mixes, and is prepared into initiation solution;
3. in the reactor with agitator, condenser, constant flow pump feeding device, 61.6g deionized water is added, be warming up to 78 DEG C, 30% of the initiation solution gross weight that 2. step is prepared is added in reactor, by the time temperature is raised to 78 again, DEG C in reactor, adds 3% of the pre-emulsion gross weight that 1. step is prepared;
4. within 3 ~ 10 minutes, in post-reactor, blue light is produced, temperature of reaction controls at 78 ~ 80 DEG C, in reactor, drip 2. remaining step prepared initiation solution and the pre-emulsion that 1. step is prepared by constant flow pump simultaneously, time for adding controlled at 2 ~ 4.5 hours, and made initiation solution add complete in 3 ~ 10 minutes after pre-emulsion dropwises;
5. temperature is risen to 90 slaking 1 ~ 2 hour, be naturally down to room temperature, filter discharging, namely obtaining band blue light solid content is 49.19%, and transformation efficiency is the conventional acrylates emulsion of 98.38%.
Comparative example 2
1. in the reactor with agitator, condenser, add the deionized water of 46.2,3.5g sodium lauryl sulphate, 0.06g lauryl mercaptan, 145g acrylate main monomer and 5.3g dibutyl itaconate, stirring at normal temperature mixes, and is prepared into pre-emulsion;
2. 0.6g Potassium Persulphate and 0.09g sodium bicarbonate are dissolved in 46.2g deionized water, stirring at normal temperature mixes, and is prepared into initiation solution;
3. in the reactor with agitator, condenser, constant flow pump feeding device, 61.6g deionized water is added, be warming up to 78, in reactor, DEG C to add the initiation solution that 2. 30% step is prepared, temperature is raised to 78 DEG C again by the time, adds the pre-emulsion that 1. 3% step is prepared in reactor;
4. within 3 ~ 10 minutes, in post-reactor, blue light is produced, temperature of reaction controls 78 ~ 80, DEG C in reactor, drip initiation solution that 2. remaining step prepared and the pre-emulsion that 1. step is prepared by constant flow pump simultaneously, time for adding controlled at 2 ~ 4.5 hours, and made initiation solution add complete in 3 ~ 10 minutes after pre-emulsion dropwises;
5. temperature is risen to 90 slaking 1 ~ 2 hour, be naturally down to room temperature, filter discharging, namely obtaining band blue light solid content is 49.04%, and transformation efficiency is the monomer modified acrylic ester emulsion of internal plasticization of 98.08%.
Comparative example 3
1. in the reactor with agitator, condenser, add 46.2g deionized water, 3.5g sodium lauryl sulphate, 0.06g lauryl mercaptan, 145g acrylate main monomer and 5.3g dibutyl maleinate, stirring at normal temperature mixes, and is prepared into pre-emulsion;
2. 0.6g Potassium Persulphate and 0.09g sodium bicarbonate are dissolved in 46.2g deionized water, stirring at normal temperature mixes, and is prepared into initiation solution;
3. in the reactor with agitator, condenser, constant flow pump feeding device, 61.6g deionized water is added, be warming up to 78 DEG C, in reactor, add the initiation solution that 2. 30% step is prepared, temperature is raised to 78 DEG C again by the time, adds the pre-emulsion that 1. 3% step is prepared in reactor;
4. within 3 ~ 10 minutes, in post-reactor, blue light is produced, temperature of reaction controls at 78 ~ 80 DEG C, in reactor, drip 2. remaining step prepared initiation solution and the pre-emulsion that 1. step is prepared by constant flow pump simultaneously, time for adding controlled at 2 ~ 4.5 hours, and made initiation solution add complete in 3 ~ 10 minutes after pre-emulsion dropwises;
5. temperature is risen to 90 DEG C of slakings 1 ~ 2 hour, be naturally down to room temperature, filter discharging, namely obtaining band blue light solid content is 48.10%, and transformation efficiency is the monomer modified acrylic ester emulsion of internal plasticization of 96.20%.
The product of the embodiment of the present invention 1 ~ 5 with comparative example 1 ~ 3 is tested under the same conditions:
The monomer modified acrylate of the internal plasticization/dilution stability of inorganic nano combined emulsion, freeze-thaw stability, mechanical stability are tested according to GB/T11175-2002, wherein mechanical stability is on supercentrifuge with the speed of rotation of 8000 rpms centrifugal 60 minutes, and whether record produces gel;
Shock resistance, glossiness are respectively by GB GB/T1732-93, GB9745-88 test;
Latex film solvent resistance is tested: 1g latex film is soaked 48 hours in sherwood oil, calculates the swelling ratio of latex film;
Latex film thermotolerance adopts DETLASWRIESTGA7 type thermogravimetric analyzer to measure, nitrogen flow 20 ml/min, temperature rise rate 10 DEG C/min, record latex film initial decomposition temperature;
Latex film tensile strength, elongation at break are tested on CMT4104 type universal electrical puller system, rate of extension 50 mm/min.Latex film intensity is reflected by the numerical value of tensile strength, and toughness is reflected by the numerical value of elongation at break.
The contrast of test gained performance perameter is as shown in table 1:
Table 1 performance perameter contrasts
Comparing embodiment 1 ~ 5 and comparative example 1 can be found out, the monomer modified acrylate of internal plasticization/inorganic nano combined emulsion has film-forming properties, solvent resistance, the shock resistance of the good dilution of conventional acrylates emulsion, freeze thawing, mechanical stability and excellence, elongation at break increases substantially, and toughness improves.
Comparing embodiment 1 ~ 5 and comparative example 2,3 can be found out, the monomer modified acrylate of internal plasticization/inorganic nano combined emulsion tensile strength increases.The present invention, by internal plasticization monomer and inorganic nano material modified acrylate, increases substantially the toughness of latex film while ensureing latex film intensity, overcomes the problem only using the monomer modified rear toughness of internal plasticization and the mutual contradiction of intensity.
Comparing embodiment 1 ~ 5 and comparative example 1 ~ 3 can be found out, the glossiness of the monomer modified acrylate of internal plasticization/inorganic nano combined emulsion latex film and thermotolerance improve, compare the monomer modified acrylic ester emulsion with internal plasticization, thermotolerance improves more obvious, widen the application category of emulsion, made it can be used as high-temperature resistant coating.
Claims (8)
1. the monomer modified acrylate of internal plasticization/inorganic nano combined emulsion, is characterized in that, its raw material is composed of the following components according to weight percent:
Wherein, described internal plasticization monomer is any one or multiple composite use in dibutyl maleinate, dibutyl itaconate, dibutyl fumarate, monobutyl itaconate, butyl maleate, dioctyl maleate;
Described inorganic nano material is any one or multiple composite use in calcium carbonate, aluminum oxide, silicon-dioxide, titanium dioxide, zinc oxide, polynite.
2. the monomer modified acrylate of internal plasticization according to claim 1/inorganic nano combined emulsion, is characterized in that, its raw material is composed of the following components according to weight percent:
3. the monomer modified acrylate of internal plasticization according to claim 1 and 2/inorganic nano combined emulsion, is characterized in that: described emulsifying agent is any one or two kinds of composite uses in allyloxy sulfated alkyl ether, polyoxyethylene alkyl ether sulfate salt, sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, alkylphenol polyoxyethylene.
4. the monomer modified acrylate of internal plasticization according to claim 1 and 2/inorganic nano combined emulsion, is characterized in that: described initiator is any one or two kinds of composite uses in ammonium persulphate, Potassium Persulphate, Potassium hydrogen sulfite, Potassium Thiosulphate.
5. the monomer modified acrylate of internal plasticization according to claim 1 and 2/inorganic nano combined emulsion, is characterized in that: described buffer reagent is any one in bicarbonate of ammonia, sodium bicarbonate, Calcium hydrogen carbonate, ammoniacal liquor.
6. the monomer modified acrylate of internal plasticization according to claim 1 and 2/inorganic nano combined emulsion, is characterized in that: described internal plasticization monomer is dibutyl itaconate or monobutyl itaconate.
7. the monomer modified acrylate of internal plasticization according to claim 1 and 2/inorganic nano combined emulsion, is characterized in that: described inorganic nano material is aluminum oxide, silicon-dioxide, titanium dioxide or zinc oxide.
8. a preparation method for the monomer modified acrylate of internal plasticization according to claim 1/inorganic nano combined emulsion, is characterized in that, comprise the following steps:
1. according to weight proportion by emulsifying agent, lauryl mercaptan, acrylate monomer and internal plasticization monomer, be added in the deionized water accounting for deionized water gross weight 20 ~ 40% used, stirring at normal temperature mixes, and is prepared into pre-emulsion;
2. initiator and buffer reagent are added in the deionized water accounting for deionized water gross weight 20 ~ 40% used, stirring at normal temperature mixes, and is prepared into initiation solution;
3. inorganic nano material is added in the deionized water accounting for deionized water gross weight 20 ~ 40% used, be warming up to that 70 ~ 85 DEG C add the initiation solution gross weight that 2. step is prepared 20 ~ 40%, by the time temperature be again raised to that 70 ~ 85 DEG C add the pre-emulsion gross weight that 1. step is prepared 3 ~ 15%;
4. blue light is produced after 3 ~ 10 minutes, temperature of reaction controls to drip initiation solution that 2. remaining step prepared and the pre-emulsion that 1. remaining step is prepared at 70 ~ 85 DEG C simultaneously, time for adding controlled at 2 ~ 4.5 hours, and made initiation solution add complete in 3-10 minute after pre-emulsion dropwises;
5. temperature is risen to 85 ~ 90 DEG C of slakings 1 ~ 2 hour, be naturally down to room temperature, filter discharging, obtain the monomer modified acrylate of internal plasticization/inorganic nano combined emulsion.
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| CN1654533A (en) * | 2005-01-19 | 2005-08-17 | 南京工业大学 | Nano silicon dioxide/acrylate composite emulsion and preparation method thereof |
| CN102020818A (en) * | 2010-11-19 | 2011-04-20 | 湖北大学 | Acrylate/silicone-acrylate compound emulsion and method for preparing same |
| CN102382506A (en) * | 2011-08-02 | 2012-03-21 | 周贤永 | Water-soluble environmentally-friendly gravure ink and preparation method thereof |
| CN102516477A (en) * | 2011-11-23 | 2012-06-27 | 华南理工大学 | Nano titanium dioxide/ acrylate composite emulsion and preparation method thereof |
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2013
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1654533A (en) * | 2005-01-19 | 2005-08-17 | 南京工业大学 | Nano silicon dioxide/acrylate composite emulsion and preparation method thereof |
| CN102020818A (en) * | 2010-11-19 | 2011-04-20 | 湖北大学 | Acrylate/silicone-acrylate compound emulsion and method for preparing same |
| CN102382506A (en) * | 2011-08-02 | 2012-03-21 | 周贤永 | Water-soluble environmentally-friendly gravure ink and preparation method thereof |
| CN102516477A (en) * | 2011-11-23 | 2012-06-27 | 华南理工大学 | Nano titanium dioxide/ acrylate composite emulsion and preparation method thereof |
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