CN108384255A - A kind of pitch releasable sbr powder microcapsules and preparation method thereof - Google Patents

A kind of pitch releasable sbr powder microcapsules and preparation method thereof Download PDF

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CN108384255A
CN108384255A CN201810105901.5A CN201810105901A CN108384255A CN 108384255 A CN108384255 A CN 108384255A CN 201810105901 A CN201810105901 A CN 201810105901A CN 108384255 A CN108384255 A CN 108384255A
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styrene
pitch
added
releasable
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CN108384255B (en
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刘清钊
马韵升
申凯华
陈梅梅
刘振学
崔丽华
张�杰
王欣
郭平云
张瑞阳
韩立霞
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Dalian University of Technology
Chambroad Chemical Industry Research Institute Co Ltd
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Dalian University of Technology
Chambroad Chemical Industry Research Institute Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L95/00Compositions of bituminous materials, e.g. asphalt, tar, pitch
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons
    • B01J13/06Making microcapsules or microballoons by phase separation
    • B01J13/14Polymerisation; cross-linking
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F112/00Homopolymers 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
    • C08F112/02Monomers containing only one unsaturated aliphatic radical
    • C08F112/04Monomers containing only one unsaturated aliphatic radical containing one ring
    • C08F112/06Hydrocarbons
    • C08F112/08Styrene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F212/00Copolymers 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
    • C08F212/02Monomers containing only one unsaturated aliphatic radical
    • C08F212/04Monomers containing only one unsaturated aliphatic radical containing one ring
    • C08F212/06Hydrocarbons
    • C08F212/08Styrene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers 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
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/14Methyl esters, e.g. methyl (meth)acrylate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/14Polymer mixtures characterised by other features containing polymeric additives characterised by shape
    • C08L2205/18Spheres

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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  • Materials Engineering (AREA)
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  • Processes Of Treating Macromolecular Substances (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Manufacturing Of Micro-Capsules (AREA)

Abstract

The present invention relates to a kind of pitch preparation methods of releasable sbr powder microcapsules.Anion styrene-butadiene latex is switched into cationic styrene-butadiene latex by transformation process first, micelle surface is set to become positively charged lotus, 100 200 μm big grain size butylbenzene micelle is formed by agglomeration process, using this butylbenzene micelle as microcapsules core material, monomer is added and is adsorbed in micelle surface, microcapsule shell is formed by graft reaction, by cohesion, pelletizes, be dried to obtain sbr powder microcapsules.The sbr powder microcapsules of preparation, which can either play isolation, prevents conglomeration, cohesion and other effects, and can be during modified pitch, and microcapsules heat shell falls off, and butadiene-styrene rubber release is swollen in pitch, plays the effect of modified pitch.

Description

A kind of pitch releasable sbr powder microcapsules and preparation method thereof
Technical field
The present invention relates to sbr powder preparing technical fields, and in particular to a kind of releasable sbr powder microcapsules of pitch And preparation method thereof.
Background technology
Currently, there are many production method of powdered rubber, include mainly mechanical crushing method, spray drying process and coacervation.But Due to the tack of rubber, the inorganic or organic interleaving agent that 20-30% is added into rubber is needed, good isolation can be just played Effect, the butadiene-styrene rubber after the cladding of physics is difficult to discharge during modified pitch use, and inorganic interleaving agent can cause The pitch uniformity declines, and seriously affects pitch low temperature ductility.There is a kind of system for the modified powder butadiene-styrene rubber introduced in patent Preparation Method includes:(1) interleaving agent used in is acidification attapulgite, is inorganic porous material;(2) interleaving agent passes through silane coupling agent It is modified, obtains siliceous attapulgite, by sufficiently large specific surface area, make isolation agent in the powdered rubber to be formed 10 parts are reduced to hereinafter, rubber content higher, more environmentally friendly.But attapulgite adsorbed close is not allowed on butadiene-styrene rubber after package Easily release, and the addition of inorganic material must influence rubber performance itself, be applied to asphalt modification, must influence pitch low temperature and prolong Malleability.
In consideration of it, invention pitch is imperative with the preparation method of releasable sbr powder microcapsules.
Invention content
For solve the prior art the above problem, the present invention provide a kind of releasable sbr powder microcapsules of pitch and its Preparation method.
To achieve the goals above, the technical solution that the application takes is as follows:
A kind of releasable sbr powder microcapsules of pitch, are prepared by each component of following heavy components:
The mass parts of dry glue are 100 parts in anionic styrene-butadiene latex;200-250 parts of deionized water;Anti-aging agent is 0.5-1 Part;4-7 parts of cationic emulsifier, 0.1-0.3 parts of colloid stabilizer;0.3-0.5 parts of electrolyte;7-10 parts of wall material monomer causes 0-0.3 parts of agent, 0.01-0.1 parts of molecular weight regulator;0.05-0.1 parts of terminator.
The pitch method of releasable sbr powder microcapsules is prepared, is as follows:
(1) anti-aging agent emulsion is prepared:0.01-0.3 parts of cationic emulsifier is weighed, 0.5-1 parts of deionized waters are added, It is heated to stirring and dissolving at 25-65 DEG C, the soap lye that mass fraction is 2-10% is configured to, anti-aging agent 0.5- is added dropwise under stirring 1 part is emulsified, and anti-aging agent emulsion mass concentration is 40-50%, ensures anti-aging agent stable homogeneous in this step;
(2) stabiliser solution is prepared:It weighs 0.1-0.3 parts of stabilizers, is added 5-15 parts of water, stirring and dissolving, in this step Ensure that stabiliser solution is uniform and stable.
(3) transition of anionic styrene-butadiene latex, agglomeration:Whole anion styrene-butadiene latexes is taken by above-mentioned parts by weight, is added It is 15-20% that deionized water, which is diluted to dry glue quality part, and 3-5 parts of cationic emulsifiers are added, and after stirring evenly, ensures fourth Benzene latex is uniform and stable, and dropwise addition mass fraction is 35-37% hydrochloric acid, and speed control 5s/d, latex pH value control is 5-6, will The anti-aging agent emulsion that step 1 is prepared all is added, and is uniformly mixing to obtain cationic styrene-butadiene latex, the stabilization prepared by step 2 Agent is all added, and (is protected to latex, 0.2-0.3 parts of electrolyte are added dropwise, carried out agglomeration, obtain 100-200 μm big grain size fourth Benzene latex;
(4) the product cation styrene-butadiene latex for obtaining step 3 is added, and in polymeric kettle, disposably adds by above-mentioned parts by weight Enter whole molecular weight regulators, residual emulsifier, 1/3-1/2 wall materials monomer, whole initiators, control temperature of reaction kettle is 60- 80 DEG C, residual monomer is added dropwise thereto, charging rate is 20 seconds/gram, reacts 1.5-2.5h, and terminator is added and stops reaction, cold But to after room temperature, being added dropwise after 0.1-0.2 part electrolyte agglomerate, granular sbr powder is obtained by cold nebulization, by vacuum It is dried to obtain butadiene-styrene rubber microcapsules.
Early period, the addition of wall material monomer was to be adsorbed in micelle surface by pre-emulsification, carries out reaction and forms wall material, due to emulsification Inefficient, the wall material thickness low LCL formed in this way is uniform, and the later stage adds wall material monomer by dropwise addition mode, be formation wall It is more uniform to form wall material thickness for the further graft reaction in material surface.
In above-mentioned preparation process, the latex that is used to prepare microcapsules is the cationic styrene-butadiene latex of transition, by agglomeration, Butylbenzene particle size analysis increases, and surface is positively charged, adsorbs wall material monomer, is closed on micelle surface under the protection of micella and stabilizer At microcapsule wall material, there is water-soluble protection gap between the microcapsule wall material and core material of formation, core material and guarantor in drying process Shield dehydration, forms " walnut " structure, under pitch heating condition, wall material falls off, and butadiene-styrene rubber is swollen in pitch, mixes, and carries High asphalt viscosity, elasticity;Wall material is fused to pitch and improves asphalt softening point.
Preferred anti-aging agent is styrenated phenol, 4- aminobphenyls, antioxidant MB, N- isopropyls-N '-phenyl to benzene two Amine, N- (1,3- dimethyl) butyl-N'- diphenyl-para-phenylene diamines, 2,2,4- trimethyl -1,2- dihyaroquinolines condensate, 4,4'- The general purpose rubbers anti-aging agents such as two (α-methylbenzyl) diphenylamines are added in styrene-butadiene latex after Over emulsfication, are uniformly dispersed, carry High rubber ageing-proof effect.
Wall material described above is thermoplastic macromolecule material, the PMMA resins of methyl methacrylate synthesis, methyl-prop Olefin(e) acid ethyl ester, methyl methacrylate synthetic resin, the styrene-acrylic resin that styrene, acrylic acid synthesize, the polyphenyl of styrene synthesis Vinyl, styrene-maleic anhydride copolymer etc..The addition of monomer secondary addition in two batches, the isolation effect of formation are more preferably micro- Capsule wall.
The stabilizer is PVA, sodium cellulose glycolate etc., and solution is formulated as 0.1-5% aqueous solutions, addition 0.1- 0.3 part.
The emulsifier is quaternary ammonium salt, imidazolines cationic emulsifier, such as hexadecyltrimethylammonium chloride, ten Eight alkyl trimethyl ammonium bromides, alkyl imidazoline quaternary ammonium salt, in three batches secondary addition, a part are antioxidant emulsion, dosage 0.02- 0.5 part;A part is that styrene-butadiene latex makes the transition, 3-5 parts of dosage;Part emulsification wall material monomer, 1-2 parts of dosage.
The electrolyte be the inorganic salts such as potassium chloride, sodium chloride, sodium bicarbonate, magnesium sulfate, calcium chloride one or more.
The initiator is heat decomposition type initiator, ammonium persulfate, the aqueous solution of potassium peroxydisulfate or hydrogen peroxide isopropyl Benzene, addition are 0-0.3 parts.
The molecular weight regulator is one kind in primary, secondary, the tertiary mercaptan, mercaptan ester and mercaptan ether of 9-14 carbon atom Or it is a variety of.
The terminator is Sodium Dimethyldithiocarbamate, sodium polysulfide.
The microcapsules are shaped to cold nebulization and obtain microcapsule granule, and drying process is 40-50 DEG C and is dried in vacuo To butadiene-styrene rubber microcapsules.
The beneficial effects of the invention are as follows:Sbr powder microcapsules are prepared by the cationic styrene-butadiene latex of transition, are passed through Agglomeration, butylbenzene particle size analysis increase, and surface is positively charged, it is easier to wall material monomer is adsorbed, under the protection of micella and stabilizer Microcapsule wall material is synthesized on micelle surface, has water-soluble protection gap between the microcapsule wall material and core material of formation, it is dried Core material and protection dehydration, form " walnut " structure, under pitch heating condition, wall material falls off, and butadiene-styrene rubber is in pitch in journey Swelling, mixing, improve asphalt viscosity, elasticity;Wall material is fused to pitch and improves asphalt softening point.
Specific implementation mode
Embodiment 1
1. anti-aging agent emulsion is prepared:0.9g hexadecyltrimethylammonium chlorides are weighed, add deionized water to 27g, heating It is dissolved to 50 DEG C, 18g antioxidant SPs is added, after stirring evenly, are configured to 40% anti-aging agent emulsion;2. weighing 571g35% Styrene-butadiene latex, be added 428g deionized waters dilution, be added 8g hexadecyltrimethylammonium chlorides, stir evenly, be added dropwise quality Score is 35-37% hydrochloric acid, and speed control 5s/d, adjustment latex pH value is 5-6, and above-mentioned 1/10 anti-aging agent emulsion is added, It is uniformly mixing to obtain cationic styrene-butadiene latex, the PVA solution of 5g4% is added, is stirred, it is attached that the 2.4g progress of 25%KCl solution is added dropwise It is poly-, obtain 100-200 μm of large-particle-size styrene-butadiene latex.3. large-particle-size styrene-butadiene latex is added in polymeric kettle, 3.5g hexadecanes are added Base trimethyl ammonium chloride opens stirring and 5g methyl methacrylates, 1g butyl acrylates is added, and tert-dodecyl mercaptan 0.1g is added A concentration of 3% potassium persulfate solution 6g, control temperature of reaction kettle are 70 DEG C, and 10g methyl methacrylates, 2g third are added dropwise thereto Olefin(e) acid butyl ester mixed liquor, rate of addition are 20 seconds/gram, react 1.5h, Sodium Dimethyldithiocarbamate 0.16g is added, and after being cooled to room temperature, are added dropwise 1.6g25%KCl agglomerates, and 100 DEG C of adjustment spray dryer temperature obtains granular sbr powder, by 40 DEG C of vacuum drying 4h Obtain butadiene-styrene rubber microcapsules.
Capsule particle degree is less than 1mm;Sbr powder powder formation rate 96.8%, water content 0.29%
2 polystyrene of embodiment
1. anti-aging agent emulsion is prepared:0.7g Cetyltrimethylammonium bromides are weighed, adds deionized water to 12.8g, adds Heat is added 10.5g N- (1,3- dimethyl) butyl-N'- diphenyl-para-phenylene diamines, after stirring evenly, is configured to 35 DEG C of dissolvings 45% anti-aging agent emulsion;2. weighing the styrene-butadiene latex of 571g35%, the dilution of 428g deionized waters is added, 7g octadecanes are added Base trimethylammonium bromide, stirs evenly, and dropwise addition mass fraction is 35-37% hydrochloric acid, and speed control 5s/d adjusts latex pH value For 5-6, above-mentioned 1/10 anti-aging agent emulsion is added, is uniformly mixing to obtain cationic styrene-butadiene latex, the methylol of 20g1% is added Cellulose receives solution, stirring, and 25%KCl solution 1.6g is added dropwise and carries out agglomeration, obtains 100-200 μm of large-particle-size styrene-butadiene latex.③ Large-particle-size styrene-butadiene latex is added in polymeric kettle, 4g Cetyltrimethylammonium bromides are added, stirring is opened and 5.3g benzene second is added A concentration of 3% potassium persulfate solution 10g is added in alkene, and control temperature of reaction kettle is 75 DEG C, and 10.7g styrene, drop are added dropwise thereto Acceleration is 20 seconds/gram, reacts 2h, and Sodium Dimethyldithiocarbamate 0.16g is added, and after being cooled to room temperature, the cohesion of 1.6g25% magnesium sulfate is added dropwise, adjusts 120 DEG C of whole spray dryer temperature, obtains granular sbr powder, and the micro- glue of butadiene-styrene rubber is obtained by 40 DEG C of vacuum drying 2.5h Capsule.
Capsule particle degree is less than 1mm;Sbr powder powder formation rate 98.5%, water content 0.68%
Embodiment 3
1. anti-aging agent emulsion is prepared:2.2g hexadecyltrimethylammonium chlorides are weighed, adds deionized water to 24.4g, adds Heat is added 20g antioxidant MBs, after stirring evenly, is configured to 45% anti-aging agent emulsion to 50 DEG C of dissolvings;2. weighing The styrene-butadiene latex of 571g35% is added the dilution of 428g deionized waters, 6g hexadecyltrimethylammonium chlorides is added, stir evenly, Dropwise addition mass fraction is 35-37% hydrochloric acid, and speed control 5s/d, adjustment latex pH value is 5-6, and above-mentioned 1/10 anti-aging agent is added Emulsion is uniformly mixing to obtain cationic styrene-butadiene latex, and the hydroxymethyl cellulose sodium solution of 15g2% is added, and stirs, and is added dropwise 25%NaCl solution 1.8g carries out agglomeration, obtains 100-200 μm of large-particle-size styrene-butadiene latex.3. weighing 5g maleic anhydrides, 10g benzene second Alkene, 20g acetone, 0.1g tert-dodecyl mercaptans, 0.02g initiator dicumyl peroxides are heated to 60 DEG C, pre-polymerization 15min, after cooling 40g water is added, the emulsification of 4g hexadecyltrimethylammonium chlorides is added in large-particle-size styrene-butadiene latex polymeric kettle, control reaction kettle temperature Degree is 75 DEG C, and 5g styrene is added dropwise thereto, and rate of addition is 20 seconds/gram, reacts 1h, Sodium Dimethyldithiocarbamate 0.1g is added, is cooled to room 1.6g25%CaCl is added dropwise in Wen Hou2Solution casting, 150 DEG C of adjustment spray dryer temperature, obtains granular sbr powder, passes through It crosses 40 DEG C of vacuum drying 2h and obtains butadiene-styrene rubber microcapsules.
Capsule particle degree is less than 1mm;Sbr powder powder formation rate 96.2%, water content 0.51%.
Embodiment 4
1. anti-aging agent emulsion is prepared:Weigh 1.35g N- butyl-N, N- bis- (3,-chloro- 2- hydroxypropyls) butane -1- ammoniums Salt adds deionized water to 27g, is heated to 45 DEG C of stirring and dissolvings, and 18g 4,4'- bis- (α-methylbenzyl) diphenylamines, stirring is added After uniformly, it is configured to 40% anti-aging agent emulsion;2. weighing the styrene-butadiene latex of 571g35%, it is dilute that 428g deionized waters are added It releases, 5.5g N- butyl-N, N- bis- (3,-chloro- 2- hydroxypropyls) butane -1- ammonium salts is added, stir evenly, mass fraction, which is added dropwise, is 35-37% hydrochloric acid, speed control 5s/d, adjustment latex pH value are 5-6, and above-mentioned 1/10 anti-aging agent emulsion is added, and stirring is equal It is even to obtain cationic styrene-butadiene latex, the PVA solution of 10g2% is added, stirs, 25%KCl solution 1.8g is added dropwise and carries out agglomeration, obtains To 100-200 μm of large-particle-size styrene-butadiene latex.3. large-particle-size styrene-butadiene latex is added in polymeric kettle, 3.5g N- butyl-N, N- is added Two (3,-chloro- 2- hydroxypropyls) butane -1- ammonium salts open stirring and are added 9g styrene, 2g acrylic acid, 0.05g n- dodecyl mereaptans, A concentration of 3% ammonium persulfate solution 6.7g is added, control temperature of reaction kettle is 65 DEG C, and 9g styrene is added dropwise thereto, speed is added dropwise Degree is 20 seconds/gram, reacts 2.5h, and sodium polysulfide 0.16g is added, and after being cooled to room temperature, 1.8g25%CaCl is added dropwise2Cohesion is adjusted 120 DEG C of whole spray dryer temperature, obtains granular sbr powder, and the micro- glue of butadiene-styrene rubber is obtained by 40 DEG C of vacuum drying 2h Capsule.
Capsule particle degree is less than 1mm;Sbr powder powder formation rate 99.1%, water content 0.76%.
To sbr powder microcapsules performance test of modified bitumen in the various embodiments described above, wherein performance test methods are using existing There is technology, is as follows:90# pitches are heated to 135 DEG C, 3% sbr powder microcapsules are added, are warming up to 160 DEG C Stirring swelling 1h is put into 165 DEG C of down cut 50min, latter 160 DEG C fully swelling 30mim, sample preparations on cutter and tests.The present invention The basic index of matrix pitch used is 45 DEG C of softening point, and 15 DEG C of ductility 45cm, 25 DEG C of needle penetration 95dmm, concrete outcome is such as Shown in lower:
Number Water content Softening point 5 DEG C of ductilities Needle penetration
Embodiment 1 0.29% 52.6℃ >150cm 85dmm
Embodiment 2 0.68% 51.3℃ >150cm 87dmm
Embodiment 3 0.51% 53.4℃ >150cm 81dmm
Embodiment 4 0.76% 51.8℃ >150cm 89dmm
It can be obtained according to the above results:The sbr powder Microcapsules Size prepared using the present invention is evenly distributed, and 1mm is less than, Water content is less than 1% after drying, and powder formation rate is improved by 85% to 95%, after sbr powder microencapsulation, improves matrix drip Green softening point is increased to greater than 51 DEG C by 45 DEG C, is required for (48 DEG C) more than SBR classes (II-B) standard, the glue prepared by the present invention 5 DEG C of ductilities of pitch can be increased to 150cm or more by breast, considerably beyond standard (50cm) requirement, have rubber powder Microcapsules Size It is evenly distributed, the advantages that powder formation rate is high, simple for process, energy conservation and environmental protection.
Explanation:Since aging inhibitor dosage is less, prepares anti-aging agent emulsion and be not easy to prepare, so being presented as in instances The anti-aging agent emulsion for preparing 10 times, takes 1/10 in use.

Claims (10)

1. a kind of releasable sbr powder microcapsules of pitch, which is characterized in that be prepared by each component of following heavy components:
The mass parts of dry glue are 100 parts in the anionic styrene-butadiene latex that solid content is 30~35%;Deionized water 200-250 Part;Anti-aging agent is 0.5-1 parts;4-7 parts of cationic emulsifier, 0.1-0.3 parts of stabilizer;0.3-0.5 parts of electrolyte;Wall material monomer 7-10 parts, 0-0.3 parts of initiator, 0.01-0.1 parts of molecular weight regulator;0.05-0.1 parts of terminator.
2. the method for preparing the releasable sbr powder microcapsules of pitch as described in claim 1, which is characterized in that specific step It is rapid as follows:
(1) anti-aging agent emulsion is prepared:0.01-0.3 parts of cationic emulsifier is weighed, 0.5-2 parts of deionized waters, heating is added Stirring and dissolving to 25-65 DEG C is configured to the soap lye that mass fraction is 2-10%, 0.5-1 parts of anti-aging agent is added dropwise under stirring It is emulsified, anti-aging agent emulsion mass concentration is 40-50%, ensures anti-aging agent stable homogeneous in this step;
(2) stabiliser solution is prepared:0.1-0.3 parts of stabilizers are weighed, 5-15 parts of water, stirring and dissolving is added;
(3) transition of anionic styrene-butadiene latex, agglomeration:Take whole anion styrene-butadiene latexes by above-mentioned parts by weight, addition go from It is 15-20% that sub- water, which is diluted to dry glue quality part, and 3-5 parts of cationic emulsifiers are added, and after stirring evenly, ensures butadiene-styrene rubber Breast is uniform and stable, and dropwise addition mass fraction is 35-37% hydrochloric acid, and speed control 5s/d, latex pH value control is 5-6, by step (1) the anti-aging agent emulsion prepared all is added, and is uniformly mixing to obtain cationic styrene-butadiene latex, the stabilization prepared by step (2) Agent is all added, and is protected to latex, and 0.2-0.3 parts of electrolyte are added dropwise, and carries out agglomeration, obtains 100-200 μm big grain size fourth Benzene latex;
(4) the product cation styrene-butadiene latex for obtaining step (3) is added, and in polymeric kettle, is added at one time by above-mentioned parts by weight Whole molecular weight regulators, residual emulsifier, 1/3-1/2 wall materials monomer, whole initiators, control temperature of reaction kettle are 60-80 DEG C, residual monomer is added dropwise thereto, charging rate is 20 seconds/gram, reacts 1.5-2.5h, and terminator is added and stops reaction, cooling To room temperature, after 0.1-0.2 parts of electrolyte cohesions are added dropwise, granular sbr powder is obtained by cold nebulization, it is dry by vacuum It is dry to obtain butadiene-styrene rubber microcapsules.
3. the releasable sbr powder microcapsules of pitch as described in claim 1, which is characterized in that anti-aging agent is styrol Phenol, 4- aminobphenyls, antioxidant MB, N- isopropyls-N '-diphenyl-para-phenylene diamine, N- (1,3- dimethyl) butyl-N'- phenyl One kind in p-phenylenediamine, 2,2,4- trimethyl -1,2- dihyaroquinolines condensate, 4,4'- bis- (α-methylbenzyl) diphenylamines.
4. the releasable sbr powder microcapsules of pitch as described in claim 1, which is characterized in that the wall material is methyl The PMMA resins of methyl acrylate synthesis, ethyl methacrylate, methyl methacrylate synthetic resin, styrene, acrylic acid The styrene-acrylic resin of synthesis, the polystyrene resin of styrene synthesis, one kind in styrene-maleic anhydride copolymer.
5. the releasable sbr powder microcapsules of pitch as described in claim 1, which is characterized in that the stabilizer be PVA, One kind in sodium cellulose glycolate.
6. the releasable sbr powder microcapsules of pitch as described in claim 1, which is characterized in that the emulsifier is season Ammonium salt class, imidazolines cationic emulsifier.
7. the releasable sbr powder microcapsules of pitch as described in claim 1, which is characterized in that the electrolyte is chlorination One or more in potassium, sodium chloride, sodium bicarbonate, magnesium sulfate, calcium chloride.
8. the releasable sbr powder microcapsules of pitch as described in claim 1, which is characterized in that the initiator is heat Breakdown type initiator, ammonium persulfate, potassium peroxydisulfate or cumyl hydroperoxide.
9. the releasable sbr powder microcapsules of pitch as described in claim 1, which is characterized in that the molecular-weight adjusting Agent is one or more in primary, secondary, the tertiary mercaptan, mercaptan ester and mercaptan ether of 9-14 carbon atom.
10. the releasable sbr powder microcapsules of pitch as described in claim 1, which is characterized in that the terminator is Sodium Dimethyldithiocarbamate, sodium polysulfide.
CN201810105901.5A 2018-02-02 2018-02-02 Releasable styrene-butadiene rubber powder microcapsule for asphalt and preparation method thereof Active CN108384255B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111560096A (en) * 2019-02-14 2020-08-21 中国石油天然气股份有限公司 Preparation method of styrene butadiene rubber
CN111925662A (en) * 2020-08-24 2020-11-13 山东京博中聚新材料有限公司 Polystyrene emulsion for modified emulsified asphalt and preparation method and application thereof
CN112480437A (en) * 2020-11-13 2021-03-12 天津大沽化工股份有限公司 Preparation method of large-particle-size high-solid-content styrene-butadiene latex
CN112771120A (en) * 2018-09-27 2021-05-07 巴斯夫欧洲公司 Latex styrene butadiene powder and asphalt composition comprising said powder
CN113278210A (en) * 2021-05-19 2021-08-20 山东高速集团有限公司创新研究院 Rubber-plastic alloy for modified asphalt mixture and preparation method thereof

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GB602260A (en) * 1944-10-06 1948-05-24 Standard Oil Dev Co Improved conjoint products and method of preparation thereof
CN104130587A (en) * 2014-07-21 2014-11-05 武汉理工大学 Rubber powder modified asphalt composition capsule
CN105385178A (en) * 2015-12-25 2016-03-09 长安大学 Crack pouring material capable of preventing secondary cracking of road surface and preparation method thereof
CN107400373A (en) * 2016-05-20 2017-11-28 天津圣工科技有限公司 A kind of preparation method of the high heat-resisting microcapsules of organo-mineral complexing bilayer wall material for pitch selfreparing

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Publication number Priority date Publication date Assignee Title
GB602260A (en) * 1944-10-06 1948-05-24 Standard Oil Dev Co Improved conjoint products and method of preparation thereof
CN104130587A (en) * 2014-07-21 2014-11-05 武汉理工大学 Rubber powder modified asphalt composition capsule
CN105385178A (en) * 2015-12-25 2016-03-09 长安大学 Crack pouring material capable of preventing secondary cracking of road surface and preparation method thereof
CN107400373A (en) * 2016-05-20 2017-11-28 天津圣工科技有限公司 A kind of preparation method of the high heat-resisting microcapsules of organo-mineral complexing bilayer wall material for pitch selfreparing

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112771120A (en) * 2018-09-27 2021-05-07 巴斯夫欧洲公司 Latex styrene butadiene powder and asphalt composition comprising said powder
CN111560096A (en) * 2019-02-14 2020-08-21 中国石油天然气股份有限公司 Preparation method of styrene butadiene rubber
CN111560096B (en) * 2019-02-14 2023-02-10 中国石油天然气股份有限公司 Preparation method of styrene butadiene rubber
CN111925662A (en) * 2020-08-24 2020-11-13 山东京博中聚新材料有限公司 Polystyrene emulsion for modified emulsified asphalt and preparation method and application thereof
CN112480437A (en) * 2020-11-13 2021-03-12 天津大沽化工股份有限公司 Preparation method of large-particle-size high-solid-content styrene-butadiene latex
CN112480437B (en) * 2020-11-13 2023-04-18 天津大沽化工股份有限公司 Preparation method of large-particle-size high-solid-content styrene-butadiene latex
CN113278210A (en) * 2021-05-19 2021-08-20 山东高速集团有限公司创新研究院 Rubber-plastic alloy for modified asphalt mixture and preparation method thereof

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