CN104692695A - Cationic asphalt emulsifier, and preparation method and application thereof - Google Patents
Cationic asphalt emulsifier, and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a cationic asphalt emulsifier, and a preparation method and application thereof. The cationic asphalt emulsifier comprises: a main agent, which is prepared by reacting an intermediate with a quaternary amination agent in a mol ratio of 0.5-3: 1, wherein the intermediate is prepared by reacting mixed organic acid with organic amine in a mol ratio of 1: 1-3, the mixed organic acid is a mixture of straight-chain, branch-chain or naphthenic-base-containing organic acid with small steric hinderance effect and organic acid with large steric hinderance effect in a mass ratio of 1: 3 to 3: 1, and the quaternary amination agent is epoxy chloropropane, hydrochloric acid, chloromethane, dimethylsulfate acetum or chloroacetic acid; and an auxiliary agent, which is a combination of a nonionic surfactant and a modification auxiliary agent, wherein the nonionic surfactant accounts for 0.1 to 2.5% of the weight of the main agent, the modification auxiliary agent accounts for 0.1 to 2.5% of the weight of the main agent, the modification auxiliary agent is a one or a mixture of more than one selected from the group consisting of aluminum sulfate, lead oxide and calcium oxide; and the nonionic surfactant is mainly composed of polyoxyethylene fatty alcohol. The cationic asphalt emulsifier provided by the invention has no adverse effects on asphalt properties, has wide applicability and can meet needs of different construction conditions.
Description
Technical field
The present invention relates to a kind of asphalt emulsifier and make each methods and applications, relate to a kind of cation asphalt emulgent in particular and make each methods and applications.
Background technology
Cation asphalt emulgent is various in style both at home and abroad at present, mainly contains following six types: alkyl amine, amides, imidazolines, oxyethane diamine class, aminated lignin class and quaternary ammonium salts.China starts to develop cationic emulsified bitumen in the later stage seventies, and oneself business-like kind mainly contains at present: alkyl amine, amides, imidazolines, oxyethane diamine class, aminated lignin class and quaternary ammonium salts cation asphalt emulgent.Due to these emulsifying agents only select-kind of organic acid and-kind of aminated compounds is raw material, make its product there is chemical structure imperfection, the incomplete defect of formulating of recipe, thus cause it to be only applicable to specific pitch and specific building stones.
The report of relevant amides or imidazolines cation asphalt emulgent has: Chen Yucheng, the development [J] of woods banyan light .AY-1 type cation asphalt emulgent. Guizhou University's journal, 2002; 19 (4) obtain amide intermediate with commercial grease and reacting ethylenediamine, then obtain product with hydrochloric acid is quaternized; Zhu Xianchun. cation asphalt emulgent [J]. Henan chemical industry, 1987; Propose and react by longer chain fatty acid the method producing asphalt emulsifier with many polyethylene polyamine; Ma Yanqiu, Wang Renhui. the research [J] of novel cation asphalt emulsifier. petroleum pitch, 1995; 9 (4) get naphthenic acid or Yatall MA and certain aminate react generate amides be used as asphalt emulsifier; Tang Yanhui, Shen Benxian, Yi Hongwei etc. the research of Emulsifying Effect of Asphalt Emulsifying Agents. Huadong Chemical College journal, 1993; 19 (6) condensations at 160 ~ 180 DEG C by diethylenetriamine and oleic acid, condensation product cyclisation under 190 ~ 240 DEG C of conditions, obtains amino-ethyl hydrogenation tetrahydroglyoxaline; Chinese patent CN1096714A disclose adopt naphthenic acid and alkenyl polyamine react obtained acid amides or imidazolines split soon in split type emulsifying agent, this agent hydroxyl steeps property comparatively by force, and emulsion surface skining is thicker; Patent CN1861721A discloses and reacts obtained rosin intermediate by common rosin or maleic-modified rosin and alkenyl polyamine, then obtains asphalt emulsifier product with quaternary ammonium salt intermediate condensation; US Patent No. P4338136 discloses and reacts obtained tetrahydroglyoxaline asphalt emulsifier with diethylene triamine at-fixed condition by C12-18 longer chain fatty acid.
The preparation of the emulsifying agent that above document or patent are reported, all select list-organic acid and list-organic amine to be that raw material reaction obtains, its shortcoming is that raw material is fixed, and raw material sources are limited, not enough or in short supply; In addition; due to the design of its chemical structure single-; in product, oleophilic group and space steric hindrance group are fixed; thus its emulsifying capacity and de-emulsification speed can not be regulated;-kind of emulsifier production only can for specific pitch and building stones; to the building stones of other character and the pitch bad adaptability of different varieties, show emulsifying effectiveness incessantly, the shortcoming such as bad, the emulsified bitumen of emulsified and re-cross pitch and polymer modified asphalt difficulty, stability of emulsion and building stones poor adhesion or mix performance deficiency; In addition, be difficult to adjust formula flexibly for different construction conditions and type, the technical requirements of working-yard cannot be reached.
Summary of the invention
Object of the present invention it-be to provide-kind of cation asphalt emulgent, to overcome in prior art emulsifying effectiveness incessantly, emulsified and re-cross pitch and polymer modified asphalt difficulty, stability of emulsion is bad, emulsified bitumen is with building stones poor adhesion, mix performance deficiency and be difficult to adjust formula flexibly for different construction conditions and type, the shortcomings such as the technical requirements of working-yard cannot be reached, the product obtained is even, stable, emulsify well, asphaltic nature is had no adverse effects, suitability is wide, can meet the construction requirement of pitch of different nature and dissimilar building stones.
The object of this invention is to provide-the preparation method of kind of cation asphalt emulgent, is with organic amine compound, mixed organic acid for raw material, obtained acid amides, ester class or imidazoline intermediate, then through quaterisation cation asphalt emulgent.Preparation technology is simple, and raw material is easy to get, and energy consumption is little, does not produce the three wastes, good economy performance.
Three of object of the present invention is to provide-application method of kind of cation asphalt emulgent, cationic emulsified bitumen product of different nature can adjust formula for a product flexibly according to pitch of different nature and dissimilar building stones, asphaltic nature is had no adverse effects, suitability is wide, good economy performance, can meet the application of the asphalt emulsifier of the requirement of different operating technique and execution conditions.
This asphalt emulsifier is made up of host and assistant agent, wherein host is mixed organic acid and organic amine is that raw material is prepared from, its Molecular Structure Design feature is: the straight chain moderate by molecular weight, in side chain or the mixed organic acid that is composited containing the organic acid of cycloalkyl and the larger organic acid of space steric effect, the straight chain that molecular weight is moderate, side chain or can lipophilic group be provided containing the organic acid of cycloalkyl, realize paraffinic base, the similar compatibility of intermediate base or cycloalkyl pitch, the organic acid that space steric effect is larger can produce sterically hindered, slowly requirement is split when meeting emulsified bitumen mix, by the host that the mixed organic acid of different ratios and organic amine are obtained by reacting, by the product obtained after composite with assistant agent, realize the controllable of well emulsify to various pitch and emulsified bitumen and building stones duration of mixing.This asphalt emulsifier is for different structure feature, pitch of different nature and dissimilar building stones, through the emulsifying effectiveness selecting corresponding lipophilic group to reach desirable, select the de-emulsification speed that the organic acid of suitable space steric hindrance and organic amine reach desirable, and by the nitrogen in organic amine, strong adsorption is produced to building stones, make pitch can be wrapped in stone surface closely, finally make mixed material have better physicals.
Technical scheme of the present invention is as follows:
Technical scheme provided by the invention is to provide-kind of cation asphalt emulgent product, this product host is mixed organic acid: the intermediate that organic amine is obtained by reacting for 1:1 ~ 3 in molar ratio, be the product that 0.5 ~ 3:1 reacts obtained in molar ratio by quaternizing agent and intermediate, assistant agent is combined by the non-ionic surface accounting for host weight 0.1 ~ 2.5% clean property agent and the modified additive that accounts for host weight 0.1 ~ 2.5%.
Mixed organic acid in described host be by-kind or-kind more than the less straight chain of space steric effect, side chain or containing cycloalkyl organic acid with-kind or-kind more than the larger organic acid of space steric effect form by 1:3 ~ 3:1 mixed in molar ratio.
The straight chain that described space steric effect is less, side chain or the organic acid containing cycloalkyl are lauric acid, TETRADECONIC ACID, palmitic acid, molecular-weight average are 200 ~ 520 naphthenic acid, oleic acid, stearic acid, 12-base stearic acid, tetracosanoic acid.
The organic acid that described space steric effect is larger is phenylformic acid, Whitfield's ointment, sylvic acid (R0sin acid), tall oil acid (Tall-0il fatty acid), bacterium sesame oil acid (Cast0r-0il acid), Lalgine (Alginic acid), syringic acid (Syringicacid), Xanthene-9-carboxylic acid (Xanthene-9-carb0xylic acid), 4-p t butylbenzoic acid, vanillic acid (Vani llic acid).
Organic amine in described host is diethylenetriamine, triethylene tetramine, tetraethylene pentamine, quadrol, 1, 6-hexanediamine, hexahydroaniline, N-hydroxyethyl-ethylenediamine, N, N'-dimethyl-ethylenediamine, N-methyl, N-bis--ethylamine, Trimethylamine 99, diethanolamine, trolamine, N, N-dimethyl propanol amine N, N-diethylpropanolamine, N-methyl, N-ethylol amine, N-ethyl, N-ethylol amine, N-butyl, N-ethylol amine, 1, 2-propylene diamine, 1, 3-propylene diamine, 3-(dibutyl) propylamine, 1-methylpiperazine, N, N'-bis-(aminoethyl) piperazine, N-aminoethyl piperazine, one or more component combine in rosin Amine D form.
Quaternizing agent in described host is the one in epoxy chloropropane, hydrochloric acid, methyl chloride, dimethyl sulfate vinegar, Mono Chloro Acetic Acid.
Nonionogenic tenside in described assistant agent is AE03, AE05 during aliphatic alcohol polyethenoxy is made, AE07, AE09, peregal 9, peregal 15, alkyl expect polyoxyethylene by TX-10, the 0P-10 in leading-kind or-kind more than component combine form.
Modified additive in described assistant agent is Tai-Ace S 150, oxidation mirror, in calcium oxide-kind or-kind more than component combine form.
Embodiment
The present invention by the restriction of following embodiment, can not determine concrete embodiment according to technical scheme of the present invention and practical situation.
In embodiment, detection method is " standard specification for construction and acceptance of highway asphalt pavement " TGF40-2004 standard.
Embodiment 1: by lauric acid and 4-p t butylbenzoic acid in molar ratio 1:1 mix and drop in reactor, then add and be mixed with
Machine acid mol ratio is the quadrol of 2:1, adds mixing acid and quadrol that lauric acid and 4-p t butylbenzoic acid form simultaneously
The xylene solvent of gross weight 5% and the stannous oxid catalyst of 1%, stir and be warming up to 1400C, back flow reaction 9 hours, obtain intermediate, remove wherein solvent, O.51 the intermediate after epoxy chloropropane and de-democracy solvent is reacted in molar ratio, control temperature of reaction 75 scholar 5 DEG C, 0.5 hour reaction times, obtained cation asphalt emulgent host, more composite with the Tai-Ace S 150 of the 1%OP-10 of host weight and 1%, stir-concoction 1h at 45 DEG C, obtain cation asphalt emulgent, give over to emulsion test.Asphalt emulsifier obtained above is mixed with the emulsifier aqueous solution of 4% weight, with salt acid for adjusting pH value extremely
3-4, reheats to 50-60, gets the paraffin-based asphalt accounting for emulsifier aqueous solution and paraffin-based asphalt gross weight 65%, and adds
Emulsifier aqueous solution and paraffin-based asphalt, to 140 DEG C, are prepared into emulsified bitumen by colloidal mill by heat.Through performance test data
For: emulsified bitumen is cationic, and on sieve, residual content is 0.2%, wraps area be greater than 2/3 with mineral aggregate, stable storing ' property (5d)
Being 3%, with II type grating limestone mineral aggregate mix for split type slowly, can duration of mixing be 80s, presetting period 30min, and product touches the mark requirement.
Embodiment 2: 300AH-90 pitch 60g is heated to 140 DEG C for subsequent use, again the emulsifying agent obtained by example 1 and other auxiliary materials (CaCl2,0.1g, 36% hydrochloric acid 0.3g etc.) be added in the deionized water of 4.0g, and be heated to 90 DEG C, then the heated bitumen of fusing is mixed with emulsifier solution, with the high speed homogenizing 5min of FJ-200 high speed dispersion clarifixator, namely make asphalt emulsification by bitumen emulsion.
Take 100g building stones, get-quantitative water and auxiliary agent, join in iron bowl, mix, then take-quantitative emulsified bitumen, pour in iron bowl, fully stir rapidly, and start timing, start-of-record Mixable time and molding time.
Emulsification condition: 300AH-90 pitch, pH=2, emulsification dosage is 1% ~ 2%.
Emulsifying effectiveness: emulsification is complete, respond well.
Package stability: long storage periods, without Precipitation and demulsifying phenomenon, has good stability.
Mix condition: be 28 DEG C at temperature, adds 100g building stones, 1% ~ 5% cement, 8g water, 2% ~ 5% emulsified bitumen.
Mix result: can duration of mixing be 387s, for splitting type asphalt emulsifier slowly.
Emulsifying agent has good emulsifying capacity to pitch, and the emulsified bitumen of preparation has good stability in storage.Place and aqueous phase does not occur after 8 days and pitch is separated.
Embodiment 3: bi tumenf orr oad No. 140 pitch 60g are heated to 140 DEG C for subsequent use, again the emulsifying agent obtained by example 1 and other auxiliary materials (CaCl2,0.1g, 36% hydrochloric acid 0.3g etc.) be added in the deionized water of 4.0g, and be heated to 90 DEG C, then the heated bitumen of fusing is mixed with emulsifier solution, with the high speed homogenizing 5min of FJ-200 high speed dispersion clarifixator, namely make asphalt emulsification by bitumen emulsion.
Take 100g building stones, get-quantitative water and auxiliary agent, join in iron bowl, mix, then take-quantitative emulsified bitumen, pour in iron bowl, fully stir rapidly, and start timing, start-of-record Mixable time and molding time.
Emulsification condition: No. 180, bi tumenf orr oad, pH=2, emulsification dosage is 1% ~ 2%.
Emulsifying effectiveness: emulsification is complete, respond well.
Package stability: long storage periods, without Precipitation and demulsifying phenomenon, has good stability.
Mix condition: be 25 DEG C at temperature, adds 100g building stones, 1 ~ 5% cement, 8g water, 2% ~ 5% emulsified bitumen.
Mix result: can duration of mixing be 465s, for splitting type asphalt emulsifier slowly.
Emulsifying agent (b) has good emulsifying capacity to pitch, and the emulsified bitumen of preparation has good stability in storage.Place and aqueous phase does not occur after 12 days and pitch is separated.
Above-described embodiment is only for the invention example is clearly described, and the restriction not to the invention embodiment.For those of ordinary skill in the field, other multi-form change and variations can also be made on the basis of the above description.Here exhaustive without the need to also giving all embodiments.
Claims (5)
1. a cation asphalt emulgent, it is characterized in that: host is the intermediate be obtained by reacting for 1:1 ~ 3 in molar ratio by mixed organic acid and organic amine, be the product that O.5 ~ 3:1 reacts obtained in molar ratio by quaternizing agent and intermediate, assistant agent is combined by the nonionogenic tenside accounting for host weight 0.1 ~ 2.5% and the modified additive that accounts for host weight 0.1 ~ 2.5%.
2. mixed organic acid is by the less straight chain of one or more space steric effects, side chain or forms by 1:3 ~ 3:1 mixed in molar ratio containing the organic acid of cycloalkyl and the larger organic acid of one or more space steric effects;
3. quaternizing agent is epoxy chloropropane, hydrochloric acid, methyl chloride, dimethyl sulfate vinegar or Mono Chloro Acetic Acid; Modified additive is the combination of one or more components in Tai-Ace S 150, oxidation mirror, calcium oxide.
4. nonionogenic tenside is aliphatic alcohol polyethenoxy vinegar.
5. the application of cation asphalt emulgent according to claim 1, it is characterized in that: just keep the aqueous solution that described cation asphalt emulgent is mixed with 2 ~ 4% weight, after its pH value being adjusted to 2 ~ 5 with hydrochloric acid, reheat to 40 ~ 80 DEG C, be fully mixed into by colloidal mill and the matrix pitch being heated to 130 ~ 150 DEG C the emulsified bitumen that pitch weight is 50 ~ 65%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105295068A (en) * | 2015-10-30 | 2016-02-03 | 华烁科技股份有限公司 | High-cation-degree asphalt emulsifier and application thereof |
| CN114031816A (en) * | 2021-11-24 | 2022-02-11 | 中路交科科技股份有限公司 | Efficient liquid asphalt warm-mixing agent and application method thereof |
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2013
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105295068A (en) * | 2015-10-30 | 2016-02-03 | 华烁科技股份有限公司 | High-cation-degree asphalt emulsifier and application thereof |
| CN114031816A (en) * | 2021-11-24 | 2022-02-11 | 中路交科科技股份有限公司 | Efficient liquid asphalt warm-mixing agent and application method thereof |
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Application publication date: 20150610 |