CN1349978A - Fatty acyl amine extracting and purifying process with liquefied petroleum gas - Google Patents
Fatty acyl amine extracting and purifying process with liquefied petroleum gas Download PDFInfo
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- CN1349978A CN1349978A CN 01133695 CN01133695A CN1349978A CN 1349978 A CN1349978 A CN 1349978A CN 01133695 CN01133695 CN 01133695 CN 01133695 A CN01133695 A CN 01133695A CN 1349978 A CN1349978 A CN 1349978A
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Abstract
The purification process of fatty acid amide by adopting liquefied petroleum gas as extraction solvent to extract liposoluble impurity and colouring matter being in fatty aid amide is characterized by that the total content of butane and propane as main component in the solvent must be greater than or equal to 99.8%, in which the propane and butane can be randomly proportioned. The extraction time of said process is 10-240 min., the volume ratio of material and solvent is 1:0.5-4, and extraction temp. is -5 deg.C-85 deg.C, and it utilizes the heat liberation produced when the solvent is liquified and heat absorption produced when the solvent is gasified to make heat exchange of said process. Said process can raise quality of fatty acid amide product, and the amide content can be up to above 98%.
Description
(1) technical field:
The present invention relates to the purifying technique of fatty amide.
(2) background technology:
At present, the production of fatty amide, because the restriction of production technique and condition causes product to have amide content low (about 90%), the defective that color and luster is heavy directly has influence on the quality and the application of product, has reduced the value and the competitive power of product.Traditional solvent method of purification is owing to be subjected to the influence of the physicochemical property of material, complex manufacturing, energy consumption height, efficient is low, causes investment to strengthen cost up, input-output ratio is uneconomical, so manufacturer has mostly adopted directly the way with the acid amides launch products of low levels.Though the laboratory has the ethanol of employing, ether, acetone equal solvent that fatty amide is carried out purification by liquid extraction, all fails to realize suitability for industrialized production.
(3) summary of the invention:
The present invention make use of liquefied petroleum gas as solvent, extraction oil-soluble impurities composition and pigment from fatty amide, purification fatty amide, the Technology of raising product grade.
But butane, propane arbitrary proportion in the solvent of the present invention, the two total content are finished the whole process that extracts oil-soluble impurities composition and pigment from fatty amide at normal temperatures more than 99.8%.This technology extraction time is 10-240min, and the volume ratio of material and solvent for use is 1: 0.5～4, and the heat exchange in the technology is carried out in the heat absorption when heat release when utilizing solvent liquefaction and solvent evaporation, utilizes the negative pressure in the extractor, makes material be inhaled into extractor.
Fatty amide content is reached more than 98%, and color and luster is purer, makes product quality be improved, and extract can carry out second development and utilization.This technology extraction temperature is-5 ℃～85 ℃, is applicable to the physicochemical property of fatty amide, and easy and simple to handle, technology is reliable and stable, and energy consumption is low, less investment, and solvent and product separation are easy.
(4) description of drawings:
Accompanying drawing is a process flow sheet of the present invention.Among the figure, 1 is extractor, 2 is evaporating pot, and 3 is compressor, and 4 is solvent tank, 5 is the hot hydrocarbon gas import of extractor 1,6 is the interior heat transfer tube of evaporating pot 2, and 7 is the opening for feed of extractor 1, and 8 is the bottom distiller grains outlet of extractor 1,9 is the mixing oil outlet of extractor 1,10 is the air outlet on extractor 1 top, and 11 is the mixing oil and the fresh solvent import of extractor 1, and 12 is the suction opening of compressor 3,13 is the venting port of compressor 3,14 is the air outlet of evaporating pot 2, and 15 is the bottom oil outlet of evaporating pot 2, and 16 is the mixing oil import of evaporating pot 2,17 is the import of heat transfer tube 6,18 is the outlet of heat transfer tube 6, and 19 is the solvent inlet of solvent tank 4, and 20 is the outlet of solvent tank 4,21 is the evacuation port of solvent tank 4, and a falls the cone angle number of degrees of truncated cone for the extractor bottom.
(5) embodiment:
During the operation of this process system, at first extractor 1 is taken out negative pressure, utilize the negative pressure in the extractor, material is sucked extractor through the opening for feed 7 of extractor 1, until finishing feed operation, charge amount is 50%～80% of a tank volume.Close opening for feed 7 then, carry out counter-current extraction with the pot group type extracting technological method.The extraction time of material is 10-240min, extraction temperature-5 ℃～85 ℃, and the volume ratio of material and solvent load is 1: 0.5～4, the extraction mixing oil enters evaporating pot 2 by the mixing oil outlet 9 of extractor 1 bottom and the mixing oil import 16 of evaporating pot 2.During miscella evaporation, need the air outlet 14 of evaporating pot 2 is communicated with the suction opening 12 of compressor 3, when hydro carbons thing content was less than 50ppm in the mixing oil extract in the evaporating pot 2, extract was discharged through the bottom of evaporating pot 2 oil outlet 15.Solvent vapour by compressor 3 sucking-offs, after the compressed machine compression increasing temperature and pressure, import 17 by the heat transfer tube 6 in the evaporating pot 2 enters in the heat transfer tube 6, carry out heat exchange with the mixing oil in the evaporating pot 2, the liquefaction that is condensed of the solvent vapour of heat transfer tube 6, flow out from the outlet 18 of heat transfer tube, through the import 19 inflow solvent tanks 4 of solvent tank 4.
After mixing oil in the extractor 1 in the material is drawn out of, still contain certain amount of solvent in the material, for from material, removing this part solvent, the air outlet 10 of extractor 1 is communicated with the suction opening 12 of compressor 3, the solvent evaporation of material gasification in the extractor 1, by compressor 3 sucking-offs, hydro carbons thing content reaches till 1～500ppm in material.By the solvent vapour of compressor 3 sucking-offs, after the compressed machine compression increasing temperature and pressure, the hot hydrocarbon gas import 5 by extractor 1 enters in the extractor, carries out heat exchange with material in the extractor 1.After solvent evaporation in the extractor 1 in the material is intact, open the bottom distiller grains outlet 8 of extractor 1, material is discharged from, and finishes an extraction cycle process.
Solvent evaporation in the extractor 1 in the material can be carried out simultaneously with the miscella evaporation in the evaporating pot 2, the solvent vapour that evaporates can enter compressor 3 simultaneously, solvent vapour after compressed machine 3 compressions can enter in the heat transfer tube 6 of extractor 1 and evaporating pot 2 simultaneously.
Realize when of the present invention, extractor, evaporating pot, solvent tank etc. all adopt pressurized vessel, and compressor can be selected reciprocating compressor, radial compressor or screw-type compressor for use, preferably adopts reciprocating compressor.The extractor of same structure can use 2 to 16 as required, even more, has shown two in the accompanying drawing, and the evaporating pot of same structure can use 1 to 5 as required, even more, has shown 1 in the accompanying drawing.The solvent that technology is used is liquefied petroleum gas (LPG), total content 〉=99.8% of its main component butane and propane, the content of other hydro carbons and isomer thereof≤0.2%, the content of sulphur＜0.05%, total metals＜60ppb.Liquefied petroleum gas (LPG) preferably adopts the liquefied petroleum gas (LPG) of butane content 〉=50%, the extractor charge amount is preferably a jar extracting production process volumetrical 70%, the extraction time is preferably 30～120min, extraction temperature is preferably 5-60 ℃, the volume ratio of material and solvent load is 1: 0.8～1.2, generally floods material with solvent and is as the criterion.It is straight barrel that the extractor of this technology preferably adopts top, and the bottom is for falling the structure of truncated cone, and the cone angle a of bottom cone is 40 °～90 °.When carrying out suitability for industrialized production according to the present invention, in order to raise the efficiency, cut down the consumption of energy, between extractor and evaporating pot, can increase temporary jar of extraction mixing oil, the concentration difference that makes full use of mixing oil extracts; In order to guarantee that remaining solvent can remove totally in the material, before compressor, increased vacuum pump.The variation of propane, butane component only influences the pressure of system in the solvent, to the not influence of effect of extracting of material, can adjust propane, butane component according to the variation of envrionment temperature, to control suitable pressure, improves the security of system.
During miscella evaporation in the evaporating pot, the high-temperature gas that utilizes compressor outlet makes the temperature-stable of mixing oil in the precipitation process at 30 ℃-50 ℃ to the heating of the mixing oil in the evaporating pot, to guarantee precipitation efficient.
[embodiment 1] the extraction erucicamide that make use of liquefied petroleum gas
Extraction is 90%～91% with the content of material erucicamide, is the bulk goods of diameter 1.5～3.0mm, and is general pale yellow during color and luster is white, capacity 0.5t/m
3Liquefied petroleum gas (LPG) as solvent is pure butane, and service temperature is a normal temperature, and pressure is 0.5～0.6MPa.The employing volume is 5.8m
3Extractor, material erucicamide 2.0t packs into, account for about 65% of tank volume, add solvent then, (during ordinary production, it should be the mixing oil of second time extraction of extractor, when the mixing oil mass was not enough, restock added novel solvent), until the submergence material, after surpassing material 5～15cm, stop solubilizing agent.After soaking 30min, put first pass mixing oil devaporation jar.
Then, advance second time solvent (during ordinary production, should be the mixing oil of the 3rd time extraction of extractor, when the mixing oil mass was not enough, restock adds novel solvent), behind the immersion 30min, put second time mixing oil and go temporary jar according to aforesaid operations.
Then, advance the 3rd time solvent (last all over solvent must fresh solvent) according to aforesaid operations, soak 40min after, put the 3rd time mixing oil and go temporary jar.Then, with compressor material in the extractor is carried out precipitation earlier, the high-temperature gas that utilizes compressor outlet simultaneously is to the heating of the material in the extractor, to guarantee that the temperature-stable of material in the precipitation process is at 30 ℃～40 ℃.Then by vacuum pump and compressor associating precipitation, until the pressure (gauge pressure) of extractor be-0.085～-0.09MPa till.At last, the vacuum breaker blowing, the material after the extraction is pure white vivid, and amide content is 99%, and material shapes does not change, and reaches design requirements fully.
[embodiment 2] the extraction stearic amide that make use of liquefied petroleum gas
Extraction is synthetic stearic amide with material, amide content 89～90%, and the white light yellow complexion of material color and luster, laminar, unit weight 0.5t/m
3The employing volume is 5.8m
3Extractor, material stearic amide 2.0t packs into, account for about 65% of tank volume, adding solvent then (during ordinary production, should be the mixing oil of second time extraction of extractor, when the mixing oil mass is not enough, restock adds novel solvent), until the submergence material,, stop solubilizing agent above behind the material 5-15cm.After soaking 30min, put first pass mixing oil devaporation jar.
Then, advance second time solvent (during ordinary production, should be the mixing oil of the 3rd time extraction of extractor, when the mixing oil mass was not enough, restock adds novel solvent), behind the immersion 30min, put second time mixing oil and go temporary jar according to aforesaid operations.
Advance solvent the 3rd time according to aforesaid operations then, last must be a fresh solvent all over solvent, behind the immersion 40min, puts the 3rd time mixing oil and goes temporary jar.Then, with compressor material in the extractor is carried out precipitation earlier, the high-temperature gas that utilizes compressor outlet simultaneously is to the heating of the material in the extractor, to guarantee that the temperature-stable of material in the precipitation process is at 30 ℃-40 ℃.Then by vacuum pump and compressor associating precipitation, until the pressure (gauge pressure) of extractor be-0.085～-0.09MPa till.Last vacuum breaker blowing, the material after the extraction is pure white bright gorgeous, amide content 98.6%, material shapes does not change, and reaches design requirements fully.
Wherein, as butane content 60% in the liquefied petroleum gas (LPG) of solvent, all the other 40% are propane, and service temperature is a normal temperature, pressure 0.7～0.8MPa.
[embodiment 3] the extraction amine hydroxybenzene that make use of liquefied petroleum gas
Extraction is an amine hydroxybenzene with material, amide content 91～92%, shallow white granular, capacity 0.50～0.52t/m
3The employing volume is 5.8m
3Extractor, the material 2.1t that packs into accounts for about 65% of tank volume, adding solvent then (during ordinary production, should be the mixing oil of second time extraction of extractor, when the mixing oil mass is not enough, restock adds novel solvent), after the submergence material surpasses material 5～10cm, stop solubilizing agent.Soak 30min, put first pass mixing oil devaporation jar.
Then, advance second time solvent (during ordinary production, should be the mixing oil of the 3rd time extraction of extractor, when the mixing oil mass was not enough, restock adds novel solvent), behind the immersion 30min, put second time mixing oil and go temporary jar according to aforesaid operations.
Then, advance solvent the 3rd time according to aforesaid operations, last must be a fresh solvent all over solvent, behind the immersion 40min, puts the 3rd time mixing oil and goes temporary jar.Then, with compressor material in the extractor is carried out precipitation earlier, simultaneously, the high-temperature gas that utilizes compressor outlet is to the heating of the material in the extractor, to guarantee that the temperature-stable of material in the precipitation process is at 30 ℃～40 ℃.Then by vacuum pump and compressor associating precipitation, until the pressure (gauge pressure) of extractor be-0.085～-0.09MPa till.At last, the vacuum breaker blowing, extraction back material color and luster is pure white, amide content 98.8%, material shapes does not change, and reaches design requirements fully.
Wherein, as butane content 80% in the liquefied petroleum gas (LPG) of solvent, all the other 20% are propane, and service temperature is a normal temperature, and pressure is 0.6～0.8MPa.
Claims (6)
1, a kind of solvent extration purification fatty amide technology, at first use the solvent extraction material, again material is separated with extraction liquid, remove the solvent in the material, reclaim the solvent in the extraction liquid then, it is characterized in that: the solvent that this technology is used is liquefied petroleum gas (LPG), and the heat exchange in the technology is carried out in the heat absorption when heat release when utilizing solvent liquefaction and gasification.
2, purification fatty amide technology as claimed in claim 1 is characterized in that: the liquefied petroleum gas (LPG) main component butane that technology is used and the total content of propane are no less than 99.8%, but butane and propane arbitrary proportion.
3, purification fatty amide technology as claimed in claim 1, its technology is: the material charge amount is 50%～80% of a tank volume, material and extraction solvent volume ratio are: 1: 0.5～4, the extraction time is 10-240min, extraction temperature is-5 ℃～85 ℃.
4, purification fatty amide technology as claimed in claim 1 is characterized in that: employed extractor (1) top is straight barrel in extraction material process, and the bottom is a frusto-conical configuration, and the cone angle of bottom cone (a) is 40 °～90 °.
5, purification fatty amide technology as claimed in claim 1 is characterized in that: the extractor when filling with substance, utilize the negative pressure in the extractor (1), and make material suck extractor (1).
6, purification fatty amide technology as claimed in claim 1, it is characterized in that: the solvent evaporation in the interior material of extractor (1) can and evaporating pot (2) in miscella evaporation carry out simultaneously, the solvent vapour that evaporates can enter compressor (3) simultaneously, solvent vapour after compression can enter in the heat transfer tube (6) of extractor (1) and evaporating pot (2) simultaneously.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01133695 CN1349978A (en) | 2001-11-19 | 2001-11-19 | Fatty acyl amine extracting and purifying process with liquefied petroleum gas |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 01133695 CN1349978A (en) | 2001-11-19 | 2001-11-19 | Fatty acyl amine extracting and purifying process with liquefied petroleum gas |
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| CN1349978A true CN1349978A (en) | 2002-05-22 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109370766A (en) * | 2018-10-30 | 2019-02-22 | 安阳晶森生物科技有限公司 | A kind of technique for extracting curcumin and curcuma oil from turmeric |
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2001
- 2001-11-19 CN CN 01133695 patent/CN1349978A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109370766A (en) * | 2018-10-30 | 2019-02-22 | 安阳晶森生物科技有限公司 | A kind of technique for extracting curcumin and curcuma oil from turmeric |
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