CN104498196A - Method for reducing acid value of high acid value vegetable pitch - Google Patents
Method for reducing acid value of high acid value vegetable pitch Download PDFInfo
- Publication number
- CN104498196A CN104498196A CN201410687320.9A CN201410687320A CN104498196A CN 104498196 A CN104498196 A CN 104498196A CN 201410687320 A CN201410687320 A CN 201410687320A CN 104498196 A CN104498196 A CN 104498196A
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- CN
- China
- Prior art keywords
- plant asphalt
- alcohol
- acid value
- alkali
- alkaline solution
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/02—Working-up pitch, asphalt, bitumen by chemical means reaction
- C10C3/023—Working-up pitch, asphalt, bitumen by chemical means reaction with inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C3/00—Working-up pitch, asphalt, bitumen
- C10C3/06—Working-up pitch, asphalt, bitumen by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Civil Engineering (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Working-Up Tar And Pitch (AREA)
Abstract
The invention relates to a method for reducing acid value of high acid value vegetable pitch, and the acid value of vegetable pitch is reduced by combination method of alcohol extraction after alkali treatment of vegetable pitch. In the production process of biological diesel oil and fatty acids, much by-product vegetable pitch is produced, the vegetable pitch contains free fatty acids, and can cause certain influence to subsequent production process or equipment. According to the method, the free fatty acids in the vegetable pitch are neutralized by an alkali, after standing and laying, aqueous phase is removed, the alkali is recovered, alcohol is added into oil phase for extraction, the free fatty acids which are not neutralized by the alkali are dissolved in the alcohol for reaction to produce fatty acid alkyl esters similar to the vegetable pitch, and the alcohol phase is removed by distillation for production of treated low acid value vegetable pitch.
Description
Technical field
The present invention relates to a kind of method processing plant asphalt, particularly relate to a kind of method reducing high acid value plant asphalt acid number, is with the combined method process high acid value plant asphalt of alcohol extraction after alkaline purification, the modification processing technique field of platymiscium pitch.
Background technology
Plant asphalt is the by product of production biofuel and lipid acid process, is rich in free fatty acids, not only high to the manufacturing technique requirent of derived product, affects derived product quality, and also has certain corrosion to production unit.Using plant asphalt directly as boiler oil, easily cause boiler coke, reduce boiler thermal output, and the heavy metal under high temperature in ash content is to furnace tube corrosion, has a strong impact on the work-ing life of boiler.If as binder for casting, the baked tensile strength of too high acid number to binding agent has a strong impact on.
Summary of the invention
The present invention is directed to above-mentioned problems of the prior art, a kind of method reducing high acid value plant asphalt acid number is provided, solve too high use of acid number in prior art and limit to large problem, make it to become and apply raw material widely.
Method of the present invention comprises the steps:
Plant asphalt is added alkali neutralizing treatment 20 ~ 40min at 70 ~ 90 DEG C; Gained mixture is washed, the salt that imurity-removal and reaction generate; After stratification, removing aqueous phase also reclaims alkali; At 20 ~ 40 DEG C, add alcohol again, after stirring 20 ~ 40min, steam alcohol phase and reclaim, plant asphalt modified for gained is carried out drying.
Described alkali is soluble in water or alkaline solution in plant asphalt.
Described alkaline solution comprises NaOH or KOH, and in alkaline solution, OH-ionic concn is 1mol/L ~ 5mol/L.
Described alkaline solution and the mass ratio of plant asphalt be, alkaline solution: plant asphalt=1:1 ~ 4:1.
Described alcohol is low-molecular-weight alcohols, comprises methyl alcohol, ethanol, propyl alcohol.
The plant asphalt volume ratio removing aqueous phase after the add-on of described alcohol and alkaline purification is, alcohol: plant asphalt=1:1 ~ 4:1.
Compared with prior art, the outstanding substantive distinguishing features had and significant progress are also in the present invention:
Modifying process of the present invention carries out at ambient pressure, and technique is simple, easy to operate, and only need the operations such as heating, stirring, washing, extraction and drying, process easily manipulates, and modification cost is low, easy industrial applications.
The present invention's properties-correcting agent used is industrial conventional alkali, alcohol, without expensive fine chemical product.
The waste liquid produced in process of the present invention is the aqueous solution and the alcoholic solution that contain a small amount of alkaline matter, namely can be recycled, do not pollute environment after simple process.
The present invention is through the modification to plant asphalt, effectively can reduce the acid number of plant asphalt, make it have using value widely, can be used for producing binder for casting, Rubber Softener, black printed ink, bituminous composition, surface activity carbon and boiler oil etc.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with concrete enforcement, the invention will be further described.
embodiment 1
Once to drop into 15g plant asphalt.In plant asphalt, add the NaOH solution that 20mL concentration is 2mol/L, water-bath controls temperature of reaction 80 DEG C, adds 20g distilled water after stirring 30min, stirs washing 30min at 80 DEG C.Remove aqueous phase after mixture being placed in separating funnel stratification, and reclaim alkali.In the plant asphalt after alkaline purification, add methyl alcohol, the plant asphalt volume ratio removing aqueous phase after the add-on of methyl alcohol and alkaline purification is, methyl alcohol: plant asphalt=2:1; And at 30 DEG C after heated and stirred 30min, be warming up to 80 DEG C (methyl alcohol boiling point is 64.7 DEG C), and water distilling apparatus is utilized to reclaim methyl alcohol.Plant asphalt after process is put into loft drier dry 12h at 100 DEG C, obtains improved plant pitch.
embodiment 2
Plant asphalt is added KOH alkaline solution neutralizing treatment 20min at 70 DEG C, and the mass ratio of KOH alkaline solution and plant asphalt is, KOH alkaline solution: plant asphalt=1:1, and in alkaline solution, OH-ionic concn is 1mol/L; Gained mixture is washed, the salt that imurity-removal and reaction generate; After stratification, removing aqueous phase also reclaims alkali; At 20 DEG C, add ethanol again, the plant asphalt volume ratio removing aqueous phase after the add-on of ethanol and alkaline purification is, ethanol: plant asphalt=1:1, after stirring 20min, steams alcohol phase and reclaims, plant asphalt modified for gained is carried out drying.Other step is with embodiment 1.
embodiment 3
Plant asphalt is added NaOH alkaline solution neutralizing treatment 40min at 90 DEG C, and the mass ratio of NaOH alkaline solution and plant asphalt is, NaOH alkaline solution: plant asphalt=4:1, and in alkaline solution, OH-ionic concn is 5mol/L; Gained mixture is washed, the salt that imurity-removal and reaction generate; After stratification, removing aqueous phase also reclaims alkali; At 40 DEG C, add propyl alcohol again, the plant asphalt volume ratio removing aqueous phase after the add-on of propyl alcohol and alkaline purification is, propyl alcohol: plant asphalt=4:1, after stirring 40min, steams alcohol phase and reclaims, plant asphalt modified for gained is carried out drying.Other step is with embodiment 1.
embodiment 4
Plant asphalt is added KOH alkaline solution neutralizing treatment 30min at 80 DEG C, and the mass ratio of KOH alkaline solution and plant asphalt is, KOH alkaline solution: plant asphalt=3:1, and in alkaline solution, OH-ionic concn is 3mol/L; Gained mixture is washed, the salt that imurity-removal and reaction generate; After stratification, removing aqueous phase also reclaims alkali; At 30 DEG C, add methyl alcohol again, the plant asphalt volume ratio removing aqueous phase after the add-on of methyl alcohol and alkaline purification is, methyl alcohol: plant asphalt=2:1, after stirring 30min, steams alcohol phase and reclaims, plant asphalt modified for gained is carried out drying.Other step is with embodiment 1.
The present invention reduces plant asphalt Free Fat acid content by alkali neutralization and alcohol extraction process.Use alkali in the soluble in water or plant asphalt such as NaOH, KOH as alkali treatment modifying agent.When reclaiming properties-correcting agent alkali, being used in separating funnel and separating alkaline solution after stratification to recycle.The low-molecular-weight alcohol such as methyl alcohol, ethanol, propyl alcohol are used to extract properties-correcting agent as alcohol.When reclaiming properties-correcting agent alcohol, it is characterized in that utilizing alcohol different from the boiling point of plant asphalt, by still-process realization and being separated of plant asphalt.
Alkali of the present invention is soluble in water or alkaline solution in plant asphalt.Described alcohol is low-molecular-weight alcohols.Above about specific descriptions of the present invention, be only not limited to the technical scheme described by the embodiment of the present invention for illustration of the present invention.Those of ordinary skill in the art should be appreciated that and still can modify to the present invention or equivalent replacement, to reach identical technique effect.Needs are used, all in protection scope of the present invention as long as meet.
Claims (6)
1. reduce a method for high acid value plant asphalt acid number, it is characterized in that comprising the steps, plant asphalt is added alkali neutralizing treatment 20 ~ 40min at 70 ~ 90 DEG C; Gained mixture is washed, the salt that imurity-removal and reaction generate; After stratification, removing aqueous phase also reclaims alkali; At 20 ~ 40 DEG C, add alcohol again, after stirring 20 ~ 40min, steam alcohol phase and reclaim, plant asphalt modified for gained is carried out drying.
2. a kind of method reducing high acid value plant asphalt acid number according to claim 1, is characterized in that described alkali is soluble in water or alkaline solution in plant asphalt.
3. a kind of method reducing high acid value plant asphalt acid number according to claim 2, is characterized in that described alkaline solution comprises NaOH or KOH, and in alkaline solution, OH-ionic concn is 1mol/L ~ 5mol/L.
4. a kind of method reducing high acid value plant asphalt acid number according to Claims 2 or 3, is characterized in that the mass ratio of described alkaline solution and plant asphalt is, alkaline solution: plant asphalt=1:1 ~ 4:1.
5. a kind of method reducing high acid value plant asphalt acid number according to claim 1, is characterized in that described alcohol is low-molecular-weight alcohols, comprises methyl alcohol, ethanol, propyl alcohol.
6. a kind of method reducing high acid value plant asphalt acid number according to claim 1 or 5, the plant asphalt volume ratio removing aqueous phase after it is characterized in that the add-on of described alcohol and alkaline purification is, alcohol: plant asphalt=1:1 ~ 4:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410687320.9A CN104498196B (en) | 2014-11-26 | 2014-11-26 | A kind of method for reducing high acid value plant asphalt acid number |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410687320.9A CN104498196B (en) | 2014-11-26 | 2014-11-26 | A kind of method for reducing high acid value plant asphalt acid number |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104498196A true CN104498196A (en) | 2015-04-08 |
| CN104498196B CN104498196B (en) | 2018-02-02 |
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| CN201410687320.9A Expired - Fee Related CN104498196B (en) | 2014-11-26 | 2014-11-26 | A kind of method for reducing high acid value plant asphalt acid number |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3691211A (en) * | 1970-12-07 | 1972-09-12 | Procter & Gamble | Process for preparing sterols from tall oil pitch |
| CN1301704A (en) * | 1999-12-30 | 2001-07-04 | 广东省食品工业研究所 | Method for extracting hytosterol from vegitable oil asphalt or tall oil asphalt |
| CN101381610A (en) * | 2007-09-06 | 2009-03-11 | 四川古杉油脂化学有限公司 | Method for transforming plant asphalt to good quality boiler fuel |
| CN101412745A (en) * | 2008-11-27 | 2009-04-22 | 南京工业大学 | Improved method for extracting sterol from vegetable oil asphalt |
-
2014
- 2014-11-26 CN CN201410687320.9A patent/CN104498196B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3691211A (en) * | 1970-12-07 | 1972-09-12 | Procter & Gamble | Process for preparing sterols from tall oil pitch |
| CN1301704A (en) * | 1999-12-30 | 2001-07-04 | 广东省食品工业研究所 | Method for extracting hytosterol from vegitable oil asphalt or tall oil asphalt |
| CN101381610A (en) * | 2007-09-06 | 2009-03-11 | 四川古杉油脂化学有限公司 | Method for transforming plant asphalt to good quality boiler fuel |
| CN101412745A (en) * | 2008-11-27 | 2009-04-22 | 南京工业大学 | Improved method for extracting sterol from vegetable oil asphalt |
Non-Patent Citations (1)
| Title |
|---|
| 谭明安等: "菜油沥青研制和生产情况简介", 《宇航材料工艺》 * |
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| CN104498196B (en) | 2018-02-02 |
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Granted publication date: 20180202 Termination date: 20191126 |