CN104592434A - High-solid content environment-friendly phase transition microcapsule and preparation method thereof - Google Patents
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Abstract
The invention relates to a high-solid content environment-friendly phase transition microcapsule and a preparation method thereof. The high-solid content environment-friendly phase transition microcapsule can be used in building coatings and belongs to the technical field of functional phase transition energy-storing material. The high-solid content environment-friendly phase transition microcapsule comprises following materials in parts by weight: 50-70 parts of paraffin, 15-20 parts of styrene, 5-8.5 parts of methacrylic acid, 55-82 parts deionized water, 2-4 parts anionic emulsifier, 0.5-1.5 partsnonionic emulsifier and 0.25-1 part initiator. The preparation method comprises the following steps in order: 1) pre-emulsifying, wherein the 50-70 parts of paraffin, 15-20 parts of styrene, 5-8.5 parts of methacrylic acid, 55-82 parts deionized water, 2-4 parts anionic emulsifier, 0.5-1.5 partsnonionic emulsifier and 0.25-1 part initiator are sent into a pre-emulsifying reactor to pre-emulsify for 10-40 minutes at a temperature 3-15 DEG C higher than melting point of the paraffin with dispersion at a rotate speed of 800-1200r/min to obtain pre-emulsified solution; 2) covering capsule wall and cross linking; 3) post-treatment. The melting point of the paraffin is 30-60 DEG C. The high-solid content environment-friendly phase transition microcapsule prepared by the method of the invention has improved emulsion particle dispersibility and excellent stability and acid and alkali resistances.
Description
Technical field
The present invention relates to a kind of phase-change microcapsule and preparation method thereof, particularly a kind of large arch dam environment-friendly phase change microcapsule and preparation method thereof, can be applicable to building coating, belong to functional phase-changing energy storage material technology.
Background technology
Phase change material is widely used as the hot storage medium of one, its cardinal principle utilizes phase change material absorb in phase transition process and discharge a large amount of latent heat, temperature control and energy-conservation object can be reached, but this kind of material is in phase transition process, particularly when liquid phase, be easy to flowing, be restricted in actual applications.
Phase-change microcapsule is the particle wrapped up by phase change material with polymer materials that is natural or synthesis, thus avoids the contact of phase change material and other materials.At 20 century 70s, along with the maturation of microcapsulary, phase-change microcapsule technology obtains development and application.Phase-change microcapsule is made up of cyst wall and capsule-core two portions, and capsule-core is phase change material, and common solid-liquid phase change material has crystalline hydrate salt, eutectic salt hydrate, paraffin class, polyoxyethylene glycol, straight-chain paraffin, fatty acid etc.Cyst wall is generally high molecular polymer, and what normal selection was conventional has polyureas, polymeric amide, urea-formaldehyde resin, melamine formaldehyde resin, urethane or their compound system.
In recent years, existing a large amount of report discloses phase-change microcapsule and technology of preparing thereof.2004, the people such as CN1513938A Wang Lixin adopted melamine formaldehyde resin to be wall material, and select direct-connected alkane, fatty alcohol and organic esters are phase change material, have obtained phase-change microcapsule material.2006, the people such as patent CN101045857A Wang Shu army adopt the method for interfacial polymerization and in-situ polymerization, with tolylene diisocyanate and urea-formaldehyde resin bi-material for cyst material, be phase change material with paraffin, prepared bilayered microcapsule encapsulation paraffin phase change material.2006, the CN1903971A Liu Yong people such as to stand erect adopted the method directly preparing emulsion in alkaline carbamide performed polymer, controls the shell speed of growth prepare phase-change microcapsule by controlling temperature of reaction.
In the preparation method of report phase-change microcapsule, most with melamine resin, urea-formaldehyde resin, resol is wall material, and by its Effect of Materials, in cyst wall, removing residue formaldehyde becomes inevitable.In addition, adopt the method for letex polymerization, not easily remove containing emulsifying agent impurity in obtained microcapsule, and it is normal containing APE (alkylphenol polyoxyethylene) and formaldehyde objectionable impurities in emulsifying agent, in addition, the solid content of reaction is mostly about 20%, and throughput is low.
Summary of the invention
In order to solve the above-mentioned problems in the prior art, the invention provides a kind of large arch dam environment-friendly phase change microcapsule and preparation method thereof, large arch dam environment-friendly phase change microcapsule prepared by the present invention improve the dispersiveness of emulsion particle, and have satisfactory stability and resistance to acids and bases.
Technical solution of the present invention is as follows:
One) scheme one:
A kind of large arch dam environment-friendly phase change microcapsule, it is prepared from according to following step of sequentially carrying out by the raw material of following weight proportioning:
1) pre-emulsification:
50-70 part paraffin, 15-20 part vinylbenzene, 5-8.5 part methacrylic acid, 55-82 part deionized water, 2-4 part anionic emulsifier, 0.5-1.5 part nonionic emulsifying agent and 0.25-1 part initiator are joined in pre-emulsification reactor, higher than at the temperature of melting point of paraffin wax 3-15 DEG C, under the dispersion of 800-1200r/min rotating speed, pre-emulsification 10-40 minute, obtains pre-emulsion;
2) cyst wall is coated and crosslinked:
30-45 part deionized water is added in crosslinking reaction device, be heated to 78 DEG C-82 DEG C, by step 1) pre-emulsion that obtains is added drop-wise in crosslinking reaction device, drip 50-100 minute, crosslinking reaction 5.5-6.5 hour at 78 DEG C of-82 DEG C of temperature afterwards, and start in crosslinking reaction that 2.5-3.5 is little adds 0.1-0.6 part linking agent constantly, after crosslinking reaction terminates, obtain polymer emulsion;
3) aftertreatment:
Filtering separation step 2) polymer emulsion that obtains, after washing 2-5 time, namely obtain large arch dam environment-friendly phase change microcapsule;
Described melting point of paraffin wax is 30-60 DEG C.
Described nonionic emulsifying agent adopts fatty alcohol polyethenoxy ether class.
Described cationic emulsifier adopts the salt containing propenyl.
Described initiator adopts the one in Diisopropyl azodicarboxylate, benzoyl peroxide, 2,2'-Azobis(2,4-dimethylvaleronitrile), ammonium persulphate, Potassium Persulphate.
Described linking agent adopts the one in Ethylene glycol dimethacrylate, dimethyl allene acid propylene glycol ester, tetramethylene dimethacrylate, Vinylstyrene.
Two) scheme two: a kind of preparation method for the preparation of the large arch dam environment-friendly phase change microcapsule described in scheme one, the method comprises the step that next coming in order carry out:
1) pre-emulsification:
50-70 part paraffin, 15-20 part vinylbenzene, 5-8.5 part methacrylic acid, 55-82 part deionized water, 2-4 part anionic emulsifier, 0.5-1.5 part nonionic emulsifying agent and 0.25-1 part initiator are joined in pre-emulsification reactor, higher than at the temperature of melting point of paraffin wax 3-15 DEG C, under the dispersion of 800-1200r/min rotating speed, pre-emulsification 10-40 minute, obtains pre-emulsion;
2) cyst wall is coated and crosslinked:
30-45 part deionized water is added in crosslinking reaction device, be heated to 78 DEG C-82 DEG C, by step 1) pre-emulsion that obtains is added drop-wise in crosslinking reaction device, drip 50-100 minute, crosslinking reaction 5.5-6.5 hour at 78 DEG C of-82 DEG C of temperature afterwards, and start in crosslinking reaction that 2.5-3.5 is little adds 0.1-0.6 part linking agent constantly, after crosslinking reaction terminates, obtain polymer emulsion;
3) aftertreatment:
Filtering separation step 2) polymer emulsion that obtains, after washing 2-5 time, namely obtain large arch dam environment-friendly phase change microcapsule;
Described melting point of paraffin wax is 30-60 DEG C.
Inventive principle of the present invention is as follows:
The present invention is with vinylbenzene, methacrylic acid is monomer, with containing the salt of propenyl and fatty alcohol-polyoxyethylene ether for emulsifying agent, adopt the method for letex polymerization, in reaction process, vinylbenzene and methacrylic acid move to water-direction, oily interface, synthetic polymer, successfully wrap up phase change material paraffin, and the functional group contained of the anionic emulsifier selected of large arch dam environment-friendly phase change microcapsule of the present invention and nonionic emulsifying agent can directly and monomer reaction, decrease the emulsifying agent impurity in phase-change microcapsule product, and when applying in coating, in the middle of coating, promoter action is dispersed with to phase-change microcapsule.
The cyst material of microcapsule is formed by vinylbenzene and methacrylic polymeric, and not containing formaldehyde, environmental protection more compared with traditional urea-formaldehyde resin, resol cyst wall, further reduces the generation of impurity wherein.
The present invention compared with prior art, has the following advantages:
1) phase-change microcapsule prepared of the present invention, preparation technology is simple, and production efficiency is high, more efficiently.
2) phase-change microcapsule that prepared by the present invention adopts the environment-friendly type emulsifying agent that can participate in being polymerized, and emulsifying agent participates in the polymerization process of monomer, decreases the emulsifying agent impurity in phase-change microcapsule product, improves the dispersiveness of emulsion particle.
3) cyst material of phase-change microcapsule that prepared by the present invention is formed by vinylbenzene and methacrylic polymeric, and not containing formaldehyde, environmental protection more compared with traditional urea-formaldehyde resin, resol cyst wall, further reduces the generation of impurity wherein.
4) the phase-change microcapsule particle diameter prepared is at 1-5um, can directly add in building coating, do not affect the film effect of coating, oil-proof, microcapsule stability is good, and resistance to acids and bases is good, can substantially increase the heat preservation and insulation of coating, also can be applicable to field of textiles, all respects such as military field.
5) solid content that the present invention prepares gained emulsion can reach more than 50%, and in phase-change microcapsule, core accounts for microcapsule proportion up to more than 70%, and greatly enhance productivity and the heat-insulating property of microcapsule, energy-conserving and environment-protective more, are widely used.
Embodiment
Below in conjunction with embodiment, embodiment, content of the present invention is described in detail:
(1) embodiment
A kind of large arch dam environment-friendly phase change microcapsule, it is prepared from according to following step of sequentially carrying out by the raw material of following weight proportioning:
1) pre-emulsification:
50-70 part paraffin, 15-20 part vinylbenzene, 5-8.5 part methacrylic acid, 55-82 part deionized water, 2-4 part anionic emulsifier, 0.5-1.5 part nonionic emulsifying agent and 0.25-1 part initiator are joined in pre-emulsification reactor, higher than at the temperature of melting point of paraffin wax 3-15 DEG C, under the dispersion of 800-1200r/min rotating speed, pre-emulsification 10-40 minute, obtains pre-emulsion;
2) cyst wall is coated and crosslinked:
30-45 part deionized water is added in crosslinking reaction device, be heated to 78 DEG C-82 DEG C, by step 1) pre-emulsion that obtains is added drop-wise in crosslinking reaction device, drip 50-100 minute, crosslinking reaction 5.5-6.5 hour at 78 DEG C of-82 DEG C of temperature afterwards, and start in crosslinking reaction that 2.5-3.5 is little adds 0.1-0.6 part linking agent constantly, after crosslinking reaction terminates, obtain polymer emulsion;
3) aftertreatment:
Filtering separation step 2) polymer emulsion that obtains, after washing 2-5 time, namely obtain large arch dam environment-friendly phase change microcapsule;
Described melting point of paraffin wax is 30-60 DEG C.
(2) embodiment:
Embodiment 1
A kind of large arch dam environment-friendly phase change microcapsule, it is prepared from according to following step of sequentially carrying out by the raw material of following weight proportioning:
1) pre-emulsification:
55 parts of paraffin, 19.05 parts of vinylbenzene, 6.35 parts of methacrylic acids, 60 parts of deionized waters, 3.1 parts of allyl ethers hydroxylpropyl sulfonates, 1.18 parts of isomerous tridecanol polyoxyethylene ethers and 0.5 part of Diisopropyl azodicarboxylate are joined in pre-emulsification reactor, heating in water bath to 45 DEG C, under the dispersion of 900r/min rotating speed, pre-emulsification 20 minutes, obtains pre-emulsion;
2) cyst wall is coated and crosslinked:
30 parts of deionized waters are added in crosslinking reaction device, be heated to 80 DEG C, by step 1) pre-emulsion that obtains is added drop-wise in crosslinking reaction device, drip 80 minutes, crosslinking reaction 6 hours at 80 DEG C of temperature afterwards, and start 3 in crosslinking reaction and littlely add 0.45 part of Vinylstyrene constantly, after crosslinking reaction terminates, obtain polymer emulsion;
3) aftertreatment:
Filtering separation step 2) polymer emulsion that obtains, after washing 2 times, namely obtain large arch dam environment-friendly phase change microcapsule;
Described melting point of paraffin wax is 37 DEG C.
Embodiment 2
A kind of large arch dam environment-friendly phase change microcapsule, it is prepared from according to following step of sequentially carrying out by the raw material of following weight proportioning:
1) pre-emulsification:
70 parts of paraffin, 24.25 parts of vinylbenzene, 8.08 parts of methacrylic acids, 82 parts of deionized waters, 4.0 parts of allyl ethers hydroxylpropyl sulfonates, 1.5 parts of isomerous tridecanol polyoxyethylene ethers and 1 part of Diisopropyl azodicarboxylate are joined in pre-emulsification reactor, heating in water bath to 50 DEG C, under the dispersion of 900r/min rotating speed, pre-emulsification 20 minutes, obtains pre-emulsion;
2) cyst wall is coated and crosslinked:
44 parts of deionized waters are added in crosslinking reaction device, be heated to 80 DEG C, by step 1) pre-emulsion that obtains is added drop-wise in crosslinking reaction device, drip 100 minutes, crosslinking reaction 6 hours at 80 DEG C of temperature afterwards, and start 3 in crosslinking reaction and littlely add 0.6 part of Ethylene glycol dimethacrylate constantly, after crosslinking reaction terminates, obtain polymer emulsion;
3) aftertreatment:
Filtering separation step 2) polymer emulsion that obtains, after washing 2 times, namely obtain large arch dam environment-friendly phase change microcapsule;
Described melting point of paraffin wax is 42 DEG C.
Embodiment 3
A kind of large arch dam environment-friendly phase change microcapsule, it is prepared from according to following step of sequentially carrying out by the raw material of following weight proportioning:
1) pre-emulsification:
50 parts of paraffin, 15.87 parts of vinylbenzene, 5.37 parts of methacrylic acids, 54 parts of deionized waters, 3.5 parts of allyl ethers hydroxylpropyl sulfonates, 0.8 part of isomerous tridecanol polyoxyethylene ether and 0.25 part of benzoyl peroxide are joined in pre-emulsification reactor, heating in water bath to 45 DEG C, under the dispersion of 900r/min rotating speed, pre-emulsification 20 minutes, obtains pre-emulsion;
2) cyst wall is coated and crosslinked:
30 parts of deionized waters are added in crosslinking reaction device, be heated to 80 DEG C, by step 1) pre-emulsion that obtains is added drop-wise in crosslinking reaction device, drip 60 minutes, crosslinking reaction 6 hours at 80 DEG C of temperature afterwards, and start 3 in crosslinking reaction and littlely add 0.35 part of Vinylstyrene constantly, after crosslinking reaction terminates, obtain polymer emulsion;
3) aftertreatment:
Filtering separation step 2) polymer emulsion that obtains, after washing 2 times, namely obtain large arch dam environment-friendly phase change microcapsule;
Described melting point of paraffin wax is 31 DEG C.
Embodiment 4
A kind of large arch dam environment-friendly phase change microcapsule, it is prepared from according to following step of sequentially carrying out by the raw material of following weight proportioning:
1) pre-emulsification:
60 parts of paraffin, 20 parts of vinylbenzene, 8 parts of methacrylic acids, 55 parts of deionized waters, 2.8 parts of allyl ethers hydroxylpropyl sulfonates, 1.5 parts of isomerous tridecanol polyoxyethylene ethers and 0.5 part of benzoyl peroxide are joined in pre-emulsification reactor, heating in water bath to 50 DEG C, under the dispersion of 900r/min rotating speed, pre-emulsification 20 minutes, obtains pre-emulsion;
2) cyst wall is coated and crosslinked:
30 parts of deionized waters are added in crosslinking reaction device, be heated to 80 DEG C, by step 1) pre-emulsion that obtains is added drop-wise in crosslinking reaction device, drip 60 minutes, crosslinking reaction 6 hours at 80 DEG C of temperature afterwards, and start 3 in crosslinking reaction and littlely add 0.35 part of Ethylene glycol dimethacrylate constantly, after crosslinking reaction terminates, obtain polymer emulsion;
3) aftertreatment:
Filtering separation step 2) polymer emulsion that obtains, after washing 2 times, namely obtain large arch dam environment-friendly phase change microcapsule;
Described melting point of paraffin wax is 45 DEG C.
Embodiment 5
A kind of large arch dam environment-friendly phase change microcapsule, it is prepared from according to following step of sequentially carrying out by the raw material of following weight proportioning:
1) pre-emulsification:
50 parts of paraffin, 20 parts of vinylbenzene, 8 parts of methacrylic acids, 65 parts of deionized waters, 3.1 parts of allyl ethers hydroxylpropyl sulfonates, 1.08 parts of isomerous tridecanol polyoxyethylene ethers and 0.5 part of Diisopropyl azodicarboxylate are joined in pre-emulsification reactor, heating in water bath to 45 DEG C, under the dispersion of 900r/min rotating speed, pre-emulsification 20 minutes, obtains pre-emulsion;
2) cyst wall is coated and crosslinked:
35 parts of deionized waters are added in crosslinking reaction device, be heated to 80 DEG C, by step 1) pre-emulsion that obtains is added drop-wise in crosslinking reaction device, drip 60 minutes, crosslinking reaction 6 hours at 80 DEG C of temperature afterwards, and start 3 in crosslinking reaction and littlely add 0.35 part of Vinylstyrene constantly, after crosslinking reaction terminates, obtain polymer emulsion;
3) aftertreatment:
Filtering separation step 2) polymer emulsion that obtains, after washing 2 times, namely obtain large arch dam environment-friendly phase change microcapsule;
Described melting point of paraffin wax is 31 DEG C.
In above each embodiment:
Described nonionic emulsifying agent isomerous tridecanol polyoxyethylene ether is preferably the BC-690 that SOLVAY produces;
Described anionic emulsifier allyl ethers hydroxylpropyl sulfonate is preferably the COPS-1 that SOLVAY produces.
Described paraffin is preferably the paraffin that Runzhou, Zhenjiang Ze Zhong Wax special factory produces.
The preferred Aladdin reagent of described vinylbenzene, methacrylic acid, Diisopropyl azodicarboxylate, divinyl xylylene, vinylformic acid glycol ester.
The performance tests such as solid content, thermostability, enthalpy, size, resistance to acids and bases are carried out to prepared large arch dam environment-friendly phase change microcapsule.
Solid content is tested: the quality accurately taking blank flat disk is M
0, take about 1g sample, the quality of sample disk is pacifically M altogether
2, sample is heated 1h in 120 ± 2 DEG C of baking ovens.After in moisture eliminator, be cooled to room temperature, again weigh the quality M altogether of remaining sample and flat disk
1, all weighings are accurately to 0.1mg.
The percentage ratio (X) of solid content is calculated as follows:
X＝100×(M1-M0)/(M2-M0)
Measure twice, measurement result is averaged, and report test result is to a decimal.
Size measures: the size of observing microcapsule under a scanning electron microscope.
Heat enthalpy value measures: use differential scanning calorimeter (DSC) to test the heat enthalpy value of sample, test condition is: the sample accurately taking about 10mg, at N
2under atmosphere, select 10K/min temperature rate, probe temperature selects the useful range of-20 DEG C-100 DEG C.
Emulsion particle dispersiveness test: the placement phase-change microcapsule emulsion of 10 days of getting 30g joins in 100g finished product emulsion paint, stirs 30 minutes with the rotating speed of 900r/min.Get the emulsion paint sample after mixing, link plate grindometer does fineness test.
Thermal stability is tested: use thermal gravimetric analyzer (TG) to test the heat decomposition temperature of sample, test condition is: the sample taking about 10mg, at N
2under atmosphere, select 10K/min temperature rise rate, probe temperature selects the useful range of 25 DEG C-600 DEG C.
Acid resistance is tested: in microcapsule emulsion, add hydrochloric acid regulate pH value to 3, place two days later, add about 1g sample, sample is put into 50 degrees Celsius of baking ovens 1 hour in flat disk, touch whether have oil leakage phenomenon after taking-up by feel.
Alkali resistance is tested: in microcapsule emulsion, add ammoniacal liquor regulate pH value to 10, place two days later, add about 1g sample, sample is put into 50 degrees Celsius of baking ovens 1 hour in flat disk, touch whether have oil leakage phenomenon after taking-up by feel.
Through the test to each embodiment, the detection data results of large arch dam environment-friendly phase change microcapsule of the present invention is as shown in following table:
The experimental data of each embodiment test of table one---large arch dam environment-friendly phase change microcapsule
Can as apparent from table one, various embodiments of the present invention all have good thermal stability and resistance to acids and bases under difficult environmental conditions, and size distribution is all between 1-5um, and heat enthalpy value is high, and there is satisfactory stability and resistance to acids and bases, there is good using value.
In sum, the large arch dam environment-friendly phase change microcapsule of various embodiments of the present invention have very high heat enthalpy value, therefore have good energy-storage property, have good thermal stability simultaneously.
Above-mentioned embodiment is just explained in detail technical scheme of the present invention; the present invention has more than and is only confined to above-described embodiment; those skilled in the art should be understood that; every improvement on basis of the present invention according to above-mentioned principle and spirit, substitute, all should within protection scope of the present invention.
Claims (6)
1. large arch dam environment-friendly phase change microcapsule, is characterized in that: it is prepared from according to following step of sequentially carrying out by the raw material of following weight proportioning:
1) pre-emulsification:
50-70 part paraffin, 15-20 part vinylbenzene, 5-8.5 part methacrylic acid, 55-82 part deionized water, 2-4 part anionic emulsifier, 0.5-1.5 part nonionic emulsifying agent and 0.25-1 part initiator are joined in pre-emulsification reactor, higher than at the temperature of melting point of paraffin wax 3-15 DEG C, under the dispersion of 800-1200r/min rotating speed, pre-emulsification 10-40 minute, obtains pre-emulsion;
2) cyst wall is coated and crosslinked:
30-45 part deionized water is added in crosslinking reaction device, be heated to 78 DEG C-82 DEG C, by step 1) pre-emulsion that obtains is added drop-wise in crosslinking reaction device, drip 50-100 minute, crosslinking reaction 5.5-6.5 hour at 78 DEG C of-82 DEG C of temperature afterwards, and start in crosslinking reaction that 2.5-3.5 is little adds 0.1-0.6 part linking agent constantly, after crosslinking reaction terminates, obtain polymer emulsion;
3) aftertreatment:
Filtering separation step 2) polymer emulsion that obtains, after washing 2-5 time, namely obtain large arch dam environment-friendly phase change microcapsule;
Described melting point of paraffin wax is 30-60 DEG C.
2. large arch dam environment-friendly phase change microcapsule according to claim 1, is characterized in that:
Described nonionic emulsifying agent adopts fatty alcohol polyethenoxy ether class.
3. large arch dam environment-friendly phase change microcapsule according to claim 1, is characterized in that:
Described cationic emulsifier adopts the salt containing propenyl.
4. large arch dam environment-friendly phase change microcapsule according to claim 1, is characterized in that:
Described initiator adopts the one in Diisopropyl azodicarboxylate, benzoyl peroxide, 2,2'-Azobis(2,4-dimethylvaleronitrile), ammonium persulphate, Potassium Persulphate.
5. large arch dam environment-friendly phase change microcapsule according to claim 1, is characterized in that:
Described linking agent adopts the one in Ethylene glycol dimethacrylate, dimethyl allene acid propylene glycol ester, tetramethylene dimethacrylate, Vinylstyrene.
6. for the preparation of a preparation method for the large arch dam environment-friendly phase change microcapsule described in any one of claim 1-5, it is characterized in that: described large arch dam environment-friendly phase change microcapsule are according to the following step preparation sequentially carried out:
1) pre-emulsification:
50-70 part paraffin, 15-20 part vinylbenzene, 5-8.5 part methacrylic acid, 55-82 part deionized water, 2-4 part anionic emulsifier, 0.5-1.5 part nonionic emulsifying agent and 0.25-1 part initiator are joined in pre-emulsification reactor, higher than at the temperature of melting point of paraffin wax 3-15 DEG C, under the dispersion of 800-1200r/min rotating speed, pre-emulsification 10-40 minute, obtains pre-emulsion;
2) cyst wall is coated and crosslinked:
30-45 part deionized water is added in crosslinking reaction device, be heated to 78 DEG C-82 DEG C, by step 1) pre-emulsion that obtains is added drop-wise in crosslinking reaction device, drip 50-100 minute, crosslinking reaction 5.5-6.5 hour at 78 DEG C of-82 DEG C of temperature afterwards, and start in crosslinking reaction that 2.5-3.5 is little adds 0.1-0.6 part linking agent constantly, after crosslinking reaction terminates, obtain polymer emulsion;
3) aftertreatment:
Filtering separation step 2) polymer emulsion that obtains, after washing 2-5 time, namely obtain large arch dam environment-friendly phase change microcapsule;
Described melting point of paraffin wax is 30-60 DEG C.
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| CN105859954B (en) * | 2016-05-05 | 2018-03-13 | 常熟林润氟硅材料有限公司 | A kind of preparation method of water-based matt acrylic emulsion |
| CN114653314A (en) * | 2020-12-23 | 2022-06-24 | 北京化工大学 | Method for preparing self-assembled microcapsule |
| CN115386344A (en) * | 2021-05-25 | 2022-11-25 | 中国石油天然气股份有限公司 | Paraffin-based composite phase change microcapsule and preparation method thereof |
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