CN109762353A - Winter cold-repairing material and production technology - Google Patents
Winter cold-repairing material and production technology Download PDFInfo
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Abstract
The invention discloses a kind of winter cold-repairing material and production technology, cold-repairing material includes the raw material of following parts by weight: 15 parts of cold-patch liquid, 50 parts of building stones, 30 parts of aggregate, 3 parts of miberal powder and 1 part of deodorant；Wherein, cold-patch liquid includes phenol aldehyde modified silicone resin, cold-patch feed additives, octamethylcy-clotetrasiloxane etc.；Cold-patch feed additives the preparation method comprises the following steps: southern magnolia is crushed, water heating is then added, filters to obtain the first filter residue；Sub-phosphono triamine heating is added into the first filter residue, filters to obtain the first filtrate；Water is added into the first filtrate, removes hexa-methylene phosphonic amide and water, obtains mixed liquor；S4, mixed liquor is purified with silica gel column chromatography, obtains extract；Ethylene glycol, octamethylcy-clotetrasiloxane mixing are added into extract, obtains cold-patch feed additives.The present invention makes extract and ethylene glycol be used cooperatively the cold resistant performance for effectively increasing cold-repairing material by extracting extract from southern magnolia, improves the intensity of cold-repairing material.
Description
Technical field
The present invention relates to pitch cold-repairing material technical fields.It is more particularly related to a kind of winter cold-repairing material and life
Production. art.
Background technique
For bituminous pavement with surfacing, driving is comfortable, has good damping property, noise is small.In use, road surface exists
Under the action of various natures (such as oxygen, ultraviolet light, temperature, water) and human factor, it inevitably will appear pavement performance drop
It is low, or even there is pit-hole, pit slot isostructuralism disease, the road maintenance being often used at present promotes exactly to be repaired by cold-repairing material
Mend, as a kind of new material, cold-repairing material road hollow, pit slot repairing in using very extensive, but existing cold-patch
Expect that cold resistance is poor, weather cold can be such that the cementability of cold-repairing material reduces in winter, influence the normal use of road.
Summary of the invention
It is an object of the invention to solve at least the above problems, and provide the advantages of at least will be described later.
It is a still further object of the present invention to provide a kind of winter cold-repairing material and production technologies, by mentioning from southern magnolia
Extract is taken, and extract and ethylene glycol is made to be used cooperatively the cold resistant performance for effectively increasing cold-repairing material, improves cold-repairing material
Intensity.
In order to realize these purposes and other advantages according to the present invention, a kind of winter cold-repairing material is provided, including following
The raw material of parts by weight: 15 parts of cold-patch liquid, 50 parts of building stones, 30 parts of aggregate, 3 parts of miberal powder and 1 part of deodorant；
Wherein, cold-patch liquid the preparation method comprises the following steps: by mass ratio be 1:1:10:20 phenol aldehyde modified silicone resin, cold-repairing material add
It is heated 1 hour under the conditions of adding agent, octamethylcy-clotetrasiloxane and petroleum ether are mixed to be incorporated in 45~50 DEG C, petroleum is removed under reduced pressure
Ether obtains the first mixing；Dimethicone, the 0.5 times of vegetable oil and 1 measured that 2 times of phenol aldehyde modified silicone resin gross mass are measured
The potassium chloride of times amount is mixed be incorporated in 70~75 DEG C under the conditions of heat 3 hours, 4 times of phenol aldehyde modified silicone resin gross mass amounts are then added
Interleaving agent and heated 2 hours under the conditions of 70~75 DEG C, obtain the second mixing；By mass ratio is 1:1:1:2:40:80 the
One mixing, the second mixing, the hydrochloric acid of 1M, asphaltic base ball active carbon, pitch and methanol are mixed and stirred for 15 hours, with second two
Amine adjusts PH to 6~7, and vacuum distillation removes methanol to get cold-patch liquid is arrived；
Cold-patch feed additives the preparation method comprises the following steps:
S1, southern magnolia is crushed, the water that 20 times of southern magnolia total quality amounts are then added heats 2 under the conditions of 48~50 DEG C
Hour, the first filter residue is obtained by filtration；
S2, the sub-phosphono triamine of 10 times of southern magnolia gross mass amounts is added into the first filter residue and in 230~233
It is heated 18 hours under the conditions of DEG C, the first filtrate is obtained by filtration；
S3, into the first filtrate be added 2 times of hexamethyl phosphoramide amount water, be removed under reduced pressure hexa-methylene phosphonic amide and
Water obtains mixed liquor；
S4, mixed liquor is purified with silica gel column chromatography, eluent system is methanol-ethyl acetate system, collects ethyl acetate
With methanol than the eluate for 1:7~9, and solvent is removed, obtains extract；
S5, the ethylene glycol that 0.01 times of extract gross mass amount is added into extract, 3 times of octamethylcy-clotetrasiloxanes measured
Mixing, obtains cold-patch feed additives.
Preferably, miberal powder is to be mixed according to mass ratio 1:2 by Iron Ore Powder and manganese mineral powder and be made.
Preferably, to be basalt, granite and limestone be 3:1:1 mixing according to mass ratio and be made building stones.
Preferably, deodorant is Nano titanium dioxide active material.
Preferably, vegetable oil is sunflower oil.
Preferably, interleaving agent is formamide.
Preferably, comprising the following steps:
A1, the ethyl alcohol of aggregate, building stones and 50 times of aggregate gross mass amounts is mixed, bone meal gross mass 3 is then added
Gamma-aminopropyl-triethoxy-silane mixing adds the potassium hydroxide of 0.04 times of bone meal gross mass amount and adds under the conditions of 80 DEG C
Heat 18 hours, obtains the first mixture；
A2, cold-patch liquid is added in n,N-Dimethylformamide mix, be then added ethylenediamine tetra-acetic acid and in 115~
It is heated 7 hours under the conditions of 120 DEG C, obtains the second mixture, wherein cold-patch liquid, ethylenediamine tetra-acetic acid, n,N-Dimethylformamide
Mass ratio 1:0.04:20；
A3, by the first mixture, the second mixture and miberal powder are mixed be incorporated in 135~140 DEG C under the conditions of heat 1 hour,
Then divide 5 equivalent that deodorant are added to get to winter cold-repairing material product.
The present invention is include at least the following beneficial effects:
The first, the present invention makes extract and ethylene glycol with the use of effective by extracting extract from southern magnolia
The cold resistant performance for improving cold-repairing material, improves the intensity of cold-repairing material.
The second, it is added in the preparation of cold-repairing material, by phenol aldehyde modified silicone resin, cold-patch feed additives, four silicon oxygen of prestox ring
Alkane and petroleum ether mixing, phenol aldehyde modified silicone resin can not only reduce the gap of cold-repairing material, improve the intensity of cold-repairing material, and phenol
Can react with the pitch of road pit slot side wall in aldehyde modified silicone resin containing phenolic hydroxyl group and aldehyde radical, so improve cold-repairing material with
The cementability of road；Dimethicone and vegetable oil are with the use of pitch and production equipment when on the one hand can avoid producing cold-patch liquid
Bonding, reduces the waste of cold-repairing material, on the other hand convenient for pitch is evenly dispersed.
Third, cold-patch feed additives preparation in first remove substance soluble easily in water in southern magnolia with water, make cold-repairing material
The branch of molecule is even closer in system, and porosity is reduced, and the viscosity between cold-repairing material increases；Water is added into the first filtrate,
To reduce the boiling point of hexa-methylene phosphonic amide, convenient for hexa-methylene phosphonic amide is removed；Second is dissolved with octamethylcy-clotetrasiloxane
Two pure and mild extracts, a large amount of phosphine rouge are contained in extract, and a small amount of ethylene glycol can avoid the phosphatide quilt under cryogenic conditions in extract
It destroys, while reducing ethylene glycol usage amount, the freexing tolerance energy of cold-repairing material can be further enhanced.
4th, in the production technology of cold-repairing material product, three second of γ-aminopropyl is added into bone meal, interleaving agent and ethyl alcohol
Oxysilane and potassium hydroxide make aggregate, interleaving agent be thoroughly dispersed in the ethanol solution containing gamma-aminopropyl-triethoxy-silane
In, potassium hydroxide is then added, forms polysiloxane polymer, aggregate, interleaving agent is made to be dispersed in polysiloxane polymer
In, it avoids aggregate and cold-repairing material from being detached from, improves the cementability of cold-repairing material；Ethylenediamine tetra-acetic acid is added into system, can make eight first
Basic ring tetrasiloxane and gamma-aminopropyl-triethoxy-silane form resin, increase the intensity of cold-repairing material, while ethylenediamine tetra-acetic acid
It can make silicon oil solidifying under the effect of phenol aldehyde modified silicone resin, silicone oil is avoided to influence the solidification of cold-repairing material.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Specific embodiment
The present invention will be further described in detail below with reference to the embodiments, to enable those skilled in the art referring to specification
Text can be implemented accordingly.
<embodiment 1>
Winter cold-repairing material, the raw material including following parts by weight: 15 parts of cold-patch liquid, 50 parts of building stones, 30 parts of aggregate, miberal powder 3
Part and 1 part of deodorant；
Wherein, cold-patch liquid the preparation method comprises the following steps: by mass ratio be 1:1:10:20 phenol aldehyde modified silicone resin, cold-repairing material add
It is heated 1 hour under the conditions of adding agent, octamethylcy-clotetrasiloxane and petroleum ether are mixed to be incorporated in 45~50 DEG C, petroleum is removed under reduced pressure
Ether obtains the first mixing；Dimethicone, the 0.5 times of vegetable oil and 1 measured that 2 times of phenol aldehyde modified silicone resin gross mass are measured
The potassium chloride of times amount is mixed be incorporated in 70~75 DEG C under the conditions of heat 3 hours, 4 times of phenol aldehyde modified silicone resin gross mass amounts are then added
Interleaving agent and heated 2 hours under the conditions of 70~75 DEG C, obtain the second mixing；By mass ratio is 1:1:1:2:40:80 the
One mixing, the second mixing, the hydrochloric acid of 1M, asphaltic base ball active carbon, pitch and methanol are mixed and stirred for 15 hours, with second two
Amine adjusts PH to 6~7, and vacuum distillation removes methanol to get cold-patch liquid is arrived；
Cold-patch feed additives the preparation method comprises the following steps:
S1, southern magnolia is crushed, the water that 20 times of southern magnolia total quality amounts are then added heats 2 under the conditions of 48~50 DEG C
Hour, the first filter residue is obtained by filtration；
S2, the sub-phosphono triamine of 10 times of southern magnolia gross mass amounts is added into the first filter residue and in 230~233
It is heated 18 hours under the conditions of DEG C, the first filtrate is obtained by filtration；
S3, into the first filtrate be added 2 times of hexamethyl phosphoramide amount water, be removed under reduced pressure hexa-methylene phosphonic amide and
Water obtains mixed liquor；
S4, mixed liquor is purified with silica gel column chromatography, eluent system is methanol-ethyl acetate system, collects ethyl acetate
With methanol than the eluate for 1:7~9, and solvent is removed, obtains extract；
S5, the ethylene glycol that 0.01 times of extract gross mass amount is added into extract, 3 times of octamethylcy-clotetrasiloxanes measured
Mixing, obtains cold-patch feed additives.
Miberal powder is to be mixed according to mass ratio 1:2 by Iron Ore Powder and manganese mineral powder and be made.
Building stones, which are basalt, granite and limestone, to be 3:1:1 mixing according to mass ratio and is made.
Deodorant is Nano titanium dioxide active material.
Vegetable oil is sunflower oil.
Interleaving agent is formamide.
The production technology of winter cold-repairing material, comprising the following steps:
A1, the ethyl alcohol of aggregate, building stones and 50 times of aggregate gross mass amounts is mixed, bone meal gross mass 3 is then added
Gamma-aminopropyl-triethoxy-silane mixing adds the potassium hydroxide of 0.04 times of bone meal gross mass amount and adds under the conditions of 80 DEG C
Heat 18 hours, obtains the first mixture；
A2, cold-patch liquid is added in n,N-Dimethylformamide mix, be then added ethylenediamine tetra-acetic acid and in 115~
It is heated 7 hours under the conditions of 120 DEG C, obtains the second mixture, wherein cold-patch liquid, ethylenediamine tetra-acetic acid, n,N-Dimethylformamide
Mass ratio 1:0.04:20；
A3, by the first mixture, the second mixture and miberal powder are mixed be incorporated in 135~140 DEG C under the conditions of heat 1 hour,
Then divide 5 equivalent that deodorant are added to get to winter cold-repairing material product.
<comparative example 1>
It carries out preparing cold-repairing material according to the formula and production technology of 1 cold-repairing material of embodiment, wherein the difference is that cold-repairing material adds
Agent is added to use the mixture of amine and tall oil.
<comparative example 2>
It carries out preparing cold-repairing material according to the formula and production technology of 1 cold-repairing material of embodiment, wherein the difference is that wide
Yulan is directly extracted using water.
<comparative example 3>
It carries out preparing cold-repairing material according to the formula and production technology of 1 cold-repairing material of embodiment, wherein the difference is that in extract
Do not add ethylene glycol.
<comparative example 4>
It carries out preparing cold-repairing material according to the formula and production technology of 1 cold-repairing material of embodiment, wherein the difference is that in cold-patch liquid
It is not added with phenol aldehyde modified silicone resin, octamethylcy-clotetrasiloxane.
<comparative example 5>
It carries out preparing cold-repairing material according to the formula and production technology of 1 cold-repairing material of embodiment, wherein the difference is that in cold-patch liquid
It is not added with dimethicone and vegetable oil.
<comparative example 6>
It carries out preparing cold-repairing material according to the formula and production technology of 1 cold-repairing material of embodiment, wherein the difference is that production technology
Cold-repairing material is prepared using common directly mixing procedure.
<comparative example 7>
It carries out preparing cold-repairing material according to the formula and production technology of 1 cold-repairing material of embodiment, wherein the difference is that production technology
In do not add ethylenediamine tetra-acetic acid.
<control group>
Commercially available cold-repairing material
<cold-repairing material performance test>
1, freezing test
5 groups of cold-repairing materials of control group, embodiment 1, comparative example 1~3 are subjected to cold resistance test.Test method is 5 groups cold
Feed supplement is respectively placed under the conditions of -10 DEG C and tests bending strength, to test whether road cold-repairing material occurs embrittlement, test result
It is as shown in table 1:
Table 1, control group, embodiment 1, comparative example 1~3 5 groups of cold-repairing materials bending strength
| Group | Flexural tensile strength/Mpa | Moment design value/GPa |
| Embodiment 1 | 27 | 13 |
| Comparative example 1 | 25 | 14 |
| Comparative example 2 | 20 | 15 |
| Comparative example 3 | 23 | 14 |
| Control group | 17 | 17 |
Comparative analysis implements the test data of 1, comparative example 1~3 and control group it is found that the flexural tensile strength of embodiment 1 is bright
The aobvious flexural tensile strength higher than comparative example 1, comparative example 2, comparative example 3 and control group, moment design value is lower than comparative example 1, right
The moment design value of ratio 2, comparative example 3 and control group, this illustrates that cold-patch feed additives prepared by the present invention can be improved
The cold tolerance of cold-repairing material.
2, Normal Temperature
6 groups of cold-repairing materials of control group, embodiment 1, comparative example 4~7 are subjected to strength test.Test method is 6 groups of cold-patches
Material is respectively placed under room temperature and tests bending strength, and test result is as shown in table 2:
Table 2, control group, embodiment 1, the bending strength of comparative example 4~7
| Group | Compression strength/Mpa | Flexural tensile strength/Mpa | Moment design value/GPa |
| Embodiment 1 | 30 | 35 | 11 |
| Comparative example 4 | 28 | 33 | 12 |
| Comparative example 5 | 27 | 32 | 13 |
| Comparative example 6 | 20 | 30 | 15 |
| Comparative example 7 | 25 | 31 | 13 |
| Control group | 17 | 28 | 16 |
Comparative analysis embodiment 1, comparative example 4, comparative example 5 and the test data of control group are it is found that resisting for embodiment 1
Compressive Strength, flexural tensile strength obviously higher than comparative example 4, the data of 5 control group of comparative example, moment design value lower than comparative example 4,
The data of comparative example 5 and control group, this shows that cold-patch liquid of the invention can increase the intensity of cold-repairing material.
Comparative analysis embodiment 1 and comparative example 6, the test data of comparative example 7 are it is found that the compression strength of embodiment 1, curved drawing
Intensity is obviously higher than the data of comparative example 6, comparative example 7 and control group, and moment design value is lower than comparative example 6, comparative example
7 and control group data, this show the production technology of cold-repairing material of the present invention be conducive to improve cold-repairing material adhesive strength.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and embodiment shown and described herein.
Claims (7)
1. winter cold-repairing material, which is characterized in that the raw material including following parts by weight: 15 parts of cold-patch liquid, 50 parts of building stones, aggregate 30
Part, 3 parts of miberal powder and 1 part of deodorant；
Wherein, cold-patch liquid the preparation method comprises the following steps: by mass ratio be the phenol aldehyde modified silicone resin of 1:1:10:20, cold-patch feed additives,
Octamethylcy-clotetrasiloxane and petroleum ether are mixed be incorporated in 45~50 DEG C under the conditions of heat 1 hour, petroleum ether is removed under reduced pressure, obtains
To the first mixing；Dimethicone, 0.5 times of vegetable oil measured and the 1 times of amount that 2 times of phenol aldehyde modified silicone resin gross mass are measured
Potassium chloride it is mixed be incorporated in 70~75 DEG C under the conditions of heat 3 hours, be then added 4 times of phenol aldehyde modified silicone resin gross mass measure every
It is heated 2 hours from agent and under the conditions of 70~75 DEG C, obtains the second mixing；Mass ratio is mixed for the first of 1:1:1:2:40:80
Material, the second mixing, the hydrochloric acid of 1M, asphaltic base ball active carbon, pitch and methanol are mixed and stirred for 15 hours, with ethylenediamine tune
PH to 6~7 is saved, vacuum distillation removes methanol to get cold-patch liquid is arrived；
Cold-patch feed additives the preparation method comprises the following steps:
S1, southern magnolia is crushed, then it is small to heat 2 under the conditions of 48~50 DEG C for the water of 20 times of southern magnolia total quality amounts of addition
When, the first filter residue is obtained by filtration；
S2, the sub-phosphono triamine of 10 times of southern magnolia gross mass amounts is added into the first filter residue and in 230~233 DEG C of items
It is heated 18 hours under part, the first filtrate is obtained by filtration；
S3, the water that 2 times of hexamethyl phosphoramide amounts are added into the first filtrate, are removed under reduced pressure hexa-methylene phosphonic amide and water, obtain
To mixed liquor；
S4, mixed liquor is purified with silica gel column chromatography, eluent system is methanol-ethyl acetate system, collects ethyl acetate and first
Alcohol removes solvent than the eluate for 1:7~9, obtains extract；
S5, the ethylene glycol that 0.01 times of extract gross mass amount is added into extract, the octamethylcy-clotetrasiloxane of 3 times of amounts are mixed
It closes, obtains cold-patch feed additives.
2. winter cold-repairing material as described in claim 1, which is characterized in that miberal powder is by Iron Ore Powder and manganese mineral powder according to mass ratio
1:2 is mixed and is made.
3. winter cold-repairing material as described in claim 1, which is characterized in that building stones are that basalt, granite and limestone are pressed
It is 3:1:1 mixing according to mass ratio and is made.
4. winter cold-repairing material as described in claim 1, which is characterized in that deodorant is Nano titanium dioxide active material.
5. winter cold-repairing material as described in claim 1, which is characterized in that vegetable oil is sunflower oil.
6. winter cold-repairing material as described in claim 1, which is characterized in that interleaving agent is formamide.
7. the production technology of winter cold-repairing material as described in any one of claims 1 to 6, which comprises the following steps:
A1, the ethyl alcohol of aggregate, building stones and 50 times of aggregate gross mass amounts is mixed, γ-ammonia of bone meal gross mass 3 is then added
Propyl-triethoxysilicane mixing, add the potassium hydroxide of 0.04 times of bone meal gross mass amount and under the conditions of 80 DEG C heating it is 18 small
When, obtain the first mixture；
A2, it will be mixed in cold-patch liquid addition n,N-Dimethylformamide, ethylenediamine tetra-acetic acid be then added and in 115~120 DEG C
Under the conditions of heat 7 hours, obtain the second mixture, wherein cold-patch liquid, ethylenediamine tetra-acetic acid, n,N-Dimethylformamide matter
Amount compares 1:0.04:20；
A3, by the first mixture, the second mixture and miberal powder are mixed be incorporated in 135~140 DEG C under the conditions of heat 1 hour, then
Deodorant are added to get to winter cold-repairing material in points of 5 times equivalent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910015901.0A CN109762353A (en) | 2019-01-08 | 2019-01-08 | Winter cold-repairing material and production technology |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910015901.0A CN109762353A (en) | 2019-01-08 | 2019-01-08 | Winter cold-repairing material and production technology |
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| CN106751976A (en) * | 2017-03-06 | 2017-05-31 | 温州程宇建设有限公司 | A kind of road cold-repairing material and preparation method thereof |
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2019
- 2019-01-08 CN CN201910015901.0A patent/CN109762353A/en active Pending
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| CN105878538A (en) * | 2009-08-12 | 2016-08-24 | M·么达萨尼 | Extract of picrorhiza kurroa for preventing, eliminating and treating DNA-based virus in human and biotechnology industry |
| CN106751976A (en) * | 2017-03-06 | 2017-05-31 | 温州程宇建设有限公司 | A kind of road cold-repairing material and preparation method thereof |
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Application publication date: 20190517 |