CN107778891A - A kind of preparation method of yittrium oxide/castor oil modified bituminous epoxy - Google Patents
A kind of preparation method of yittrium oxide/castor oil modified bituminous epoxy Download PDFInfo
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- CN107778891A CN107778891A CN201711122428.3A CN201711122428A CN107778891A CN 107778891 A CN107778891 A CN 107778891A CN 201711122428 A CN201711122428 A CN 201711122428A CN 107778891 A CN107778891 A CN 107778891A
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- castor oil
- pitch
- yittrium oxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
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- Engineering & Computer Science (AREA)
- Civil Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Epoxy Resins (AREA)
- Road Paving Structures (AREA)
Abstract
The invention discloses a kind of preparation method of yittrium oxide/castor oil modified bituminous epoxy, with raw materials such as yittrium oxide, castor oil, epoxy resin, sulphur, pitches by saponification acid hydrolyzation, application of vacuum, the methods of thermal agitation is handled synthetic castor oil modified epoxy pitch.The present invention carries out half epoxidation reaction using peroxide acid system to bulking agent presoma.When alkene is with peroxide acid oxidase, the oxygen atom in peroxy acid carries out three-dimensional single-minded cis addition with olefinic double bonds.Bulking agent makes to form chemical key connection between epoxy resin and matrix pitch, generates three-dimensional net structure by the chemical reaction such as being crosslinked, being grafted, is advantageous to obtain high performance pitch.
Description
Technical field
The present invention relates to a kind of preparation method of yittrium oxide/castor oil modified bituminous epoxy, belong to Material Field.
Background technology
Pitch is a kind of common construction material, and very important construction material.It is must not in urban construction
One of goods and materials that can be less.Due to pitch a variety of premium properties such as have resist chemical, antiseepage, waterproof, cohesion strong in itself, from
B.C. more than 3000 years by the mankind find utilize since, now to highway communication, water conservancy and hydropower, industry, building, agricultural,
The multiple fields such as coating play a significant role.The 85% of world's bituminous production is all applied in road construction, and pitch is built in road
If application technology in is also the most ripe.The raw material of current various ground surface materials is mainly cement and pitch, but pitch
Road surface has that driving comfort level is high, and noise is small, many advantages such as antiskid compared with cement pavement, so, asphalt roads in recent years
Construction it is more and more in cement pavement, the highway that especially China was built in recent years is nearly all bituminous paving.
But tensile strength of pitch etc. need to be improved at present, I have invented a kind of yittrium oxide/castor oil modified bituminous epoxy, prepares
Simply, function admirable.
The content of the invention
In view of the above-mentioned problems of the prior art, the present invention provides a kind of yittrium oxide/castor oil modified bituminous epoxy
Preparation method, the tensile strength of pitch are high.
To achieve these goals, the technical solution adopted by the present invention is a kind of yittrium oxide/castor oil modified bituminous epoxy
Preparation method.Comprise the following steps：
Step 1, a certain amount of castor oil is weighed in 250ml beaker, stirred in the water bath with thermostatic control being subsequently placed at 80 DEG C；
Step 2, with another beaker into a certain amount of sodium hydroxide is taken, add in deionized water, be configured to solution, be put into same perseverance
In tepidarium, after constant temperature, alkali lye is poured into castor oil rapidly；
Step 3, treat that reflection change clarification is to start to sample, a sample is taken every 1min later, respectively with hydroxyl waste acid iron chromogenic reaction
Judge reaction end；
Step 4, into saponification liquor add HCl to liquid in acidity, stir static, multi_layer extraction, organic phase hot wash, extremely
Washings are neutrality, dry organic phase and obtain castor oil acid crude product；
Step 5, the thick castor oil acid of acid obtained above and epoxy resin -20 and appropriate dimethylbenzene are added in three-necked flask
（Solvent）, joint test device, open heating and stirring device and carry out full esterification reaction；
Step 6, it is evaporated under reduced pressure under 95 DEG C, 0.2MPa, steams solvent and obtain bulking agent presoma；
Step 7, the bulking agent presoma of removing solvent are placed in three-necked flask, joint test device.Open heating and stirring device,
And nitrogen is passed through into three-necked flask；
Step 8, after waiting until that temperature rises to 75 DEG C of design temperature by thermometer observation, the concentrated sulfuric acid is first added dropwise in flask（Urge
Agent）Then ready formic acid is added dropwise rapidly, continues after being stirred in flask, starts that H is added dropwise into three-necked flask2O2；
Step 9, add Na2CO3The aqueous solution, until system pH value is 7.Three-necked flask is taken out, stands to liquid layered in bottle, makes
The aqueous solution is removed with separatory funnel, the bulking agent finally given is placed in eggplant-shape bottle, using Rotary Evaporators, bulking agent done
It is dry, remove residual moisture；
Step 10, pitch is heated to flowing, weighs appropriate pitch, yittrium oxide, bulking agent and vulcanizing agent sulphur are stirred
Product even, that the vulcanization regular hour is vulcanized at a proper temperature；
Step 11, epoxy resin E-44 and sulfur product are blended again, add curing agent polyamide 6 50, oxygen is can obtain after 8h
Change yttrium/castor oil modified bituminous epoxy.
Beneficial effect:A kind of preparation method of yittrium oxide/castor oil modified bituminous epoxy of the present invention.The present invention uses peroxide
Acid system carries out half epoxidation reaction to bulking agent presoma.When alkene is with peroxide acid oxidase, oxygen atom and alkene in peroxy acid
Double bond carries out three-dimensional single-minded cis addition.Bulking agent makes to form chemical key connection between epoxy resin and matrix pitch, passes through
The chemical reaction generation three-dimensional net structure such as crosslinking, grafting, is advantageous to obtain high performance pitch.Pass through heat in preparation process
Stirring, yittrium oxide modification etc. can further improve the physico-chemical property of pitch.Wherein embodiment 1 produces castor oil, yittrium oxide, drip
Green grass or young crops, vulcanizing agent 30：1:400：9 sample（Unit serving）.30 parts of castor oil, 1 part of yittrium oxide, 400 parts of pitch, 9 parts, 2 parts of vulcanizing agent
HCl, 5 parts of epoxy resin -20,50 part dimethylbenzene（Solvent）, 5 parts of sodium hydroxides, 20 parts of deionized waters, 2 parts of formic acid, 1 part dense
Sulfuric acid, 3 parts of H2O210 part Na2CO3 aqueous solution, 9 parts of vulcanizing agent sulphur, 5 parts of curing agent polyamide 6s 50.Embodiment 2 produces castor-oil plant
Oil, yittrium oxide, pitch, vulcanizing agent 22：3:420：7 sample（Unit serving）.22 parts of castor oil, 3 parts of yittrium oxide, 420 parts of pitch, sulphur
7 parts of agent.Other raw material dosages, operating procedure is as embodiment 1.Yittrium oxide/castor oil modified bituminous epoxy stretching is made
Intensity is best.
Embodiment
Embodiment 1 produces castor oil, yittrium oxide, pitch, vulcanizing agent 30：1:400：9 sample（Unit serving）.Castor oil 30
Part, 1 part of yittrium oxide, 400 parts of pitch, 9 parts of vulcanizing agent, 2 parts of HCl, 5 parts of epoxy resin -20,50 part dimethylbenzene（Solvent）, 5 parts
Sodium hydroxide, 20 parts of deionized waters, 2 parts of formic acid, 1 part of concentrated sulfuric acid, 3 parts of H2O2
10 parts of Na2CO3 aqueous solution, 9 parts of vulcanizing agent sulphur, 5 parts of curing agent polyamide 6s 50.
Step 1,30 parts of castor oil are weighed in beaker, stirred in the water bath with thermostatic control being subsequently placed at 80 DEG C；
Step 2, with another beaker into 5 parts of sodium hydroxides are taken, add in 20 parts of deionized waters, be configured to solution, be put into same perseverance
In tepidarium, after constant temperature, alkali lye is poured into castor oil rapidly；
Step 3, treat that reflection change clarification is to start to sample, a sample is taken every 1min later, respectively with hydroxyl waste acid iron chromogenic reaction
Judge reaction end；
Step 4,2 parts of HCl are added to liquid in acidity into saponification liquor, stir static, multi_layer extraction, organic phase hot water wash
Wash, be neutrality to washings, dry organic phase and obtain castor oil acid crude product；
Step 5, the thick castor oil of acid obtained above and 5 parts of epoxy resins -20 and 50 parts of dimethylbenzene are added in three-necked flask
（Solvent）, joint test device, open heating and stirring device and carry out full esterification reaction；
Step 6, it is evaporated under reduced pressure under 95 DEG C, 0.2MPa, steams solvent and obtain bulking agent presoma；
Step 7, the bulking agent presoma of removing solvent are placed in three-necked flask, joint test device.Open heating and stirring device,
And nitrogen is passed through into three-necked flask；
Step 8, after waiting until that temperature rises to 75 DEG C of design temperature by thermometer observation, 1 part of concentrated sulfuric acid is first added dropwise in flask
（Catalyst）Then ready 2 parts of formic acid is added dropwise rapidly, continues after being stirred in flask, starts to drip into three-necked flask
Add 3 parts of H2O2；
Step 9,10 parts of Na2CO3 aqueous solution are added, until system pH value is 7.Three-necked flask is taken out, is stood to liquid in bottle point
Layer, the aqueous solution is removed using separatory funnel, the bulking agent finally given is placed in eggplant-shape bottle, using Rotary Evaporators, to increasing
Hold agent to dry, remove residual moisture；
Step 10,400 parts of pitches are heated to flowing, by pitch, 1 part of yittrium oxide, obtained bulking agent and 9 parts of vulcanizing agent sulphur
It is uniformly mixed, the product that the vulcanization regular hour is vulcanized at a proper temperature；
Step 11,20 parts of epoxy resin E-44s and sulfur product are blended again, 5 parts of curing agent polyamide 6s 50 of addition, after 8h
Obtain yittrium oxide/castor oil modified bituminous epoxy.
Embodiment 2 produces castor oil, yittrium oxide, pitch, vulcanizing agent 22：3:420：7 sample（Unit serving）.Castor oil 22
Part, 3 parts of yittrium oxide, 420 parts of pitch, 7 parts of vulcanizing agent.Other raw material dosages, operating procedure is as embodiment 1.
Embodiment 3 produces castor oil, yittrium oxide, pitch, vulcanizing agent 32：1:400：9 sample（Unit serving）.Castor oil 32
Part, 1 part of yittrium oxide, 400 parts of pitch, 9 parts of vulcanizing agent.Other raw material dosages, operating procedure is as embodiment 1.
Embodiment 4 produces castor oil, yittrium oxide, pitch, vulcanizing agent 34：1:400：9 sample（Unit serving）.Castor oil 34
Part, 1 part of yittrium oxide, 400 parts of pitch, 9 parts of vulcanizing agent.Other raw material dosages, operating procedure is as embodiment 1.
Embodiment 5 produces castor oil, yittrium oxide, pitch, vulcanizing agent 36：1:400：9 sample（Unit serving）.Castor oil 36
Part, 1 part of yittrium oxide, 400 parts of pitch, 9 parts of vulcanizing agent.Other raw material dosages, operating procedure is as embodiment 1.
Embodiment 6 produces castor oil, yittrium oxide, pitch, vulcanizing agent 38：1:400：9 sample（Unit serving）.Castor oil 30
Part, 1 part of yittrium oxide, 400 parts of pitch, 9 parts of vulcanizing agent.Other raw material dosages, operating procedure is as embodiment 1.
Embodiment 7 produces castor oil, yittrium oxide, pitch, vulcanizing agent 30：1.5:400：9 sample（Unit serving）.Castor oil 30
Part, 1.5 parts of yittrium oxide, 400 parts of pitch, 9 parts of vulcanizing agent.Other raw material dosages, operating procedure is as embodiment 1.
Embodiment 8 produces castor oil, yittrium oxide, pitch, vulcanizing agent 30：2:400：9 sample（Unit serving）.Castor oil 30
Part, 2 parts of yittrium oxide, 400 parts of pitch, 9 parts of vulcanizing agent.Other raw material dosages, operating procedure is as embodiment 1.
Embodiment 9 produces castor oil, yittrium oxide, pitch, vulcanizing agent 30：2.5:400：9 sample（Unit serving）.Castor oil 30
Part, 2.5 parts of yittrium oxide, 400 parts of pitch, 9 parts of vulcanizing agent,.Other raw material dosages, operating procedure is as embodiment 1.
Embodiment 10 produces castor oil, yittrium oxide, pitch, vulcanizing agent 30：1:410：9 sample（Unit serving）.Castor oil 30
Part, 1 part of yittrium oxide, 410 parts of pitch, 9 parts of vulcanizing agent,.Other raw material dosages, operating procedure is as embodiment 1.
Embodiment 11 produces castor oil, yittrium oxide, pitch, vulcanizing agent 30：1:420：9 sample（Unit serving）.Castor oil 30
Part, 1 part of yittrium oxide, 420 parts of pitch, 9 parts of vulcanizing agent,.Other raw material dosages, operating procedure is as embodiment 1.
Embodiment 12 produces castor oil, yittrium oxide, pitch, vulcanizing agent 30：1:430：9 sample（Unit serving）.Castor oil 30
Part, 1 part of yittrium oxide, 430 parts of pitch, 9 parts of vulcanizing agent.Other raw material dosages, operating procedure is as embodiment 1.
Embodiment 13 produces castor oil, yittrium oxide, pitch, vulcanizing agent 30：1:440：9 sample（Unit serving）.Castor oil 30
Part, 1 part of yittrium oxide, 400 parts of pitch, 9 parts of vulcanizing agent.Other raw material dosages, operating procedure is as embodiment 1.
Reference examples 1 produce castor oil, yittrium oxide, pitch, vulcanizing agent 30：1:400：9 sample（Unit serving）.Castor oil 30
Part, 1 part of yittrium oxide, 400 parts of pitch, 9 parts of vulcanizing agent.Wherein not to castor oil carry out water bath with thermostatic control processing, other raw material dosages,
Operating procedure is as embodiment 1.
Reference examples 2 produce castor oil, yittrium oxide, pitch, vulcanizing agent 30：1:400：9 sample（Unit serving）.Castor oil 30
Part, 1 part of yittrium oxide, 400 parts of pitch, 9 parts of vulcanizing agent.Alkali process, other raw material dosages, operation step are not carried out to castor oil wherein
Suddenly as embodiment 1.
Reference examples 3 produce castor oil, yittrium oxide, pitch, vulcanizing agent 30：1:400：9 sample（Unit serving）.30 parts of castor oil, oxygen
Change 1 part of yttrium, 400 parts of pitch, 9 parts of vulcanizing agent.Wherein without being evaporated under reduced pressure, other raw material dosages, operating procedure is with embodiment 1
Equally.
Reference examples 4 produce castor oil, yittrium oxide, pitch, vulcanizing agent 30：1:400：9 sample（Unit serving）.Castor oil 30
Part, 1 part of yittrium oxide, 400 parts of pitch, 9 parts of vulcanizing agent.Without H2O2, operating procedure is as embodiment 1.
Reference examples 5 produce yittrium oxide, pitch, vulcanizing agent 1:400：9 sample（Unit serving）.1 part of yittrium oxide, 400 parts of pitch,
9 parts of vulcanizing agent.Castor oil is wherein added without, other raw material dosages, operating procedure is as embodiment 1.
Reference examples 6 produce castor oil, pitch, vulcanizing agent 30：400：9 sample（Unit serving）.30 parts of castor oil, pitch 400
Part, 9 parts of vulcanizing agent.Yittrium oxide is wherein added without, other raw material dosages, operating procedure is as embodiment 1.
Tensile strength is tested：By pitch, epoxy resin, bulking agent, vulcanizing agent and curing agent according to made of different outfits
Yittrium oxide/castor oil modified bituminous epoxy, it is evenly coated in when not yet reaching solidification temperature on the iron plate of ground smooth, by two pieces
Iron plate is glutinous together, and two untouchable contacts area are 4 × 4cm.Isothermal curing in baking oven is put into, it is to try that solidification is taken out after terminating
Sample.Herein according to the method for ASTMD638-03 defineds, GP-TS20009 tensile testing machines are used with 500mm/min speed,
Test temperature is 20 DEG C, and sample determines tensile strength under the same conditions.
The tensile strength test results of table one
Test result indicates that：It can be found that comparative example, embodiment 1, yittrium oxide made from 2/castor oil modified bituminous epoxy
Tensile property is best.Illustrate that the raw material proportioning has preferably to act synergistically, operating procedure is good most beneficial for synthesis tensile property
Yittrium oxide/castor oil modified bituminous epoxy.Obtained yittrium oxide/castor oil modified bituminous epoxy tensile property under other techniques
Performance is general.Comparative example 1, comparative example 1,2,3,4,5,6 are can be found that.Castor oil carries out water bath with thermostatic control processing, castor oil
Alkali process is carried out, is evaporated under reduced pressure, adds H2O2, and castor oil is added, and yittrium oxide is added for obtained yittrium oxide/castor-oil plant
Oily modified epoxy pitch tensile property has tremendous influence, and overall coordination, which acts on, causes bituminous epoxy to have extraordinary stretching
Performance.
Claims (2)
1. the preparation method of a kind of yittrium oxide/castor oil modified bituminous epoxy, it is characterised in that with yittrium oxide, castor oil, epoxy
The methods of raw materials such as resin, sulphur, pitch are by saponification acid hydrolyzation, application of vacuum, and thermal agitation is handled synthetic castor oil is modified ring
Oxygen pitch.
A kind of 2. preparation method of yittrium oxide/castor oil modified bituminous epoxy:It is characterised in that it includes following steps
Step 1, a certain amount of castor oil is weighed in beaker, stirred in the water bath with thermostatic control being subsequently placed at 80 DEG C；
Step 2, with another beaker into a certain amount of sodium hydroxide is taken, add in deionized water, be configured to solution, be put into same perseverance
In tepidarium, after constant temperature, alkali lye is poured into castor oil rapidly；
Step 3, treat that reflection change clarification is to start to sample, a sample is taken every 1min later, respectively with hydroxyl waste acid iron chromogenic reaction
Judge reaction end；
Step 4, into saponification liquor add HCl to liquid in acidity, stir static, multi_layer extraction, organic phase hot wash, extremely
Washings are neutrality, dry organic phase and obtain castor oil acid crude product；
Step 5, the thick castor oil acid of acid obtained above and epoxy resin -20 and appropriate dimethylbenzene are added in three-necked flask,
Joint test device, open heating and stirring device and carry out full esterification reaction；
Step 6, it is evaporated under reduced pressure under 95 DEG C, 0.2MPa, steams solvent and obtain bulking agent presoma；
Step 7, the bulking agent presoma of removing solvent are placed in three-necked flask, joint test device, open heating and stirring device,
And nitrogen is passed through into three-necked flask；
Step 8, after waiting until that temperature rises to 75 DEG C of design temperature by thermometer observation, the concentrated sulfuric acid first is added dropwise then in flask
Ready formic acid is added dropwise rapidly, continues after being stirred in flask, starts that H2O2 is added dropwise into three-necked flask；
Step 9, the Na2CO3 aqueous solution is added, until system pH value is 7, takes out three-necked flask, stand to liquid layered in bottle, make
The aqueous solution is removed with separatory funnel, the bulking agent finally given is placed in eggplant-shape bottle, using Rotary Evaporators, bulking agent done
It is dry, remove residual moisture；
Step 10, pitch is heated to flowing, weighs appropriate pitch, yittrium oxide, bulking agent and vulcanizing agent sulphur are stirred
Product even, that the vulcanization regular hour is vulcanized at a proper temperature；
Step 11, epoxy resin E-44 and sulfur product are blended again, add curing agent polyamide 6 50, oxygen is can obtain after 8h
Change yttrium/castor oil modified bituminous epoxy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711122428.3A CN107778891A (en) | 2017-11-14 | 2017-11-14 | A kind of preparation method of yittrium oxide/castor oil modified bituminous epoxy |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711122428.3A CN107778891A (en) | 2017-11-14 | 2017-11-14 | A kind of preparation method of yittrium oxide/castor oil modified bituminous epoxy |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276790A (en) * | 2011-08-10 | 2011-12-14 | 武汉工程大学 | Method for preparing bulking agent of epoxy resin modified asphalt |
| CN102964856A (en) * | 2012-12-20 | 2013-03-13 | 中国林业科学研究院林产化学工业研究所 | Preparation method of bio-based solubilizing and toughening agent-modified epoxy asphalt material |
| CN104744953A (en) * | 2015-04-01 | 2015-07-01 | 武汉工程大学 | Thermosetting eleostearic acid ester epoxy asphalt compatibilizer and preparation method thereof |
-
2017
- 2017-11-14 CN CN201711122428.3A patent/CN107778891A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276790A (en) * | 2011-08-10 | 2011-12-14 | 武汉工程大学 | Method for preparing bulking agent of epoxy resin modified asphalt |
| CN102964856A (en) * | 2012-12-20 | 2013-03-13 | 中国林业科学研究院林产化学工业研究所 | Preparation method of bio-based solubilizing and toughening agent-modified epoxy asphalt material |
| CN104744953A (en) * | 2015-04-01 | 2015-07-01 | 武汉工程大学 | Thermosetting eleostearic acid ester epoxy asphalt compatibilizer and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 陈栋: "蓖麻油改性环氧沥青的制备及研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
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