CN101942008B - Process for extracting phytosterol from papermaking wood pulp oil slick pitch - Google Patents
Process for extracting phytosterol from papermaking wood pulp oil slick pitch Download PDFInfo
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- CN101942008B CN101942008B CN201010268028A CN201010268028A CN101942008B CN 101942008 B CN101942008 B CN 101942008B CN 201010268028 A CN201010268028 A CN 201010268028A CN 201010268028 A CN201010268028 A CN 201010268028A CN 101942008 B CN101942008 B CN 101942008B
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Abstract
The invention discloses a process for extracting phytosterol from papermaking wood pulp oil slick pitch. The method comprises the following steps of: selecting the waste of wood pulp used in the papermaking industry, i.e. wood pulp oil slick pitch; and directly extracting phytosterol from the wood pulp oil slick pitch by utilizing an ion exchange resin method. The invention can be used for directly extracting the phytosterol from the papermaking wood pulp oil slick pitch instead of the steps of extracting tall oil from the wood pulp and then extracting the phytosterol from the tall oil and has the advantages of low raw material cost, high comprehensive utilization degree and high purity and yield of the extracted phytosterol.
Description
Technical field
The invention discloses a kind of method from papermaking tall oil bitumen extraction plant sterol.
Background technology
Plant sterol is the one type of natural constituents that is present in the plant; A large amount of experimentation on animalies and human clinical trial's data show; Plant sterol and ester are a kind of important medical material and protective foods batchings for reducing blood middle cholesterol content, alleviating cardiovascular disorder generation significance.
The product B enecol that Finland Rasio company will contain plant sterol nineteen ninety-five introduces to the market; Be the country that releases plant sterol reducing cholesterol functional food in the world the earliest, have the product of countries such as Australia, Belgium, Brazil, Denmark, France, Germany, Japan, Holland, Spain, Switzerland, Sweden, Britain, the U.S. to go on the market successively later on.Plant sterol food began to get into American market in 1999, and the health bulletin of U.S. FDA issue is claimed: " plant sterol and ester can reach the effect of obvious reducing cholesterol through the reduction blood cholesterol level ".FDA permission food coating materials can add 20% saturated plant sterol.Japan approval in 1999 plant sterol and ester are the functional additive of the particular private protective foods FOSHU of regulating blood fat, and there is the food of many interpolation plant sterols in market, like oleomargarine, mayonnaise, sauce etc.Assistant rattan food company releases the packing rice that adds plant sterol recently, and every part of heavy 160g of rice has added the 3.75g plant sterol, and the plant sterol consistency is good, can also prevent the rice adhesion, improves mouthfeel.In September, 2000; The food that plant sterol and stanol ester have been added in U.S. food and Drug Administration (FDA) approval can use " good for health " label; Heath food portion of U.S. Cargill Inc. has released the plant sterol product that extracts from natural goods during the international food additive exhibition of Shanghai in March, 2006; Explanation can be added in the food such as beverage, fruit juice, sour milk, and allows in food product pack, to use the claiming of " helping to reduce coronary heart disease danger " of FDA regulation.August in 2007, Finland on the 20th Raisio Benecol Ltd. released reducing cholesterol that has and the phytostanols that promotes health of heart in Beijing; It joins in the food such as butter, cream cheese, sour milk, milk, beverage, flour products, candy, biscuit, chocolate as a kind of new type functional food additive and batching; And easy to process, do not influence the mouthfeel of food, safe; Has no spinoff; And the safe qualification (G RAS) of acquisition U.S. FDA, by the assessment approval of food authorities of European Union, the said firm actively declares to department of Chinese government concerned.
At present, the main source of plant sterol is to extract in the by product from the vegetable oil refining process, because vegetable oil refining by product output is little, price is high, the development of the severe inhibition industry at present.Therefore, the substitute that people urgently seek out the vegetable oil refining by product extracts plant sterol, and is just becoming present research focus from tall oil bitumen extraction plant sterol.
Open from the sixties in last century and to cheat, the research of extracting plant sterol the pitch scum silica frost soap of the tall oil that American-European countries is carrying out processing from tall oil always.
Early stage research mainly concentrates on the extracting and separating; People such as Johansson remove the hexane extraction method of sterol from thick sulfur soap scum silica frost; Oy Kaukas utilizes the solvent mixture separating plant sterol from soap that contains hexane, acetone, first alcohol and water; That people such as Kutney utilize is moisture, solvent mixture separating plant sterol from soap of ketone, hydrocarbon, and people such as Jullan provide through extraction in water-alcohol-hydrocarbon mixture, saponification and purifying then, from the method for tall oil bitumen production sterol.
No matter adopt single-solvent process or mixed solvent method from tall oil bitumen extraction plant sterol, all can't overcome long-chain alcohol and acidic impurities and from sterol, be difficult to isolating characteristics; In order to overcome the deficiency of solvent extration; People begin to introduce the distillatory method in the recent period, and people such as Diaz and Michael .E. Shu Erci adopt the separation method of first saponification, redistillation, back extraction, and the purity of sterol and yield obtain bigger change like this; But also there is the big contaminate environment of saponified amount; Common distillation temperature is high, and the part sterol is destroyed, and the purity of plant sterol does not reach the shortcomings such as standard of Europe, U.S. man.
In addition; From tall oil pitch, prepare plant sterol, with regard to basic material, must be containing the higher timber of oil slick through leaching; Extract tall oil pitch; Only this step has just been expended many human and material resources, financial resources, and sterol extraction process afterwards also exists above-mentioned many defectives, thereby we must study according to China's raw material resources and industriallization emphasis.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, select for use used wood pulp in the paper industry waste---tall oil pitch is raw material, directly from tall oil pitch, extract the method for plant sterol.
The present invention realizes through following technical scheme: a kind of method of from papermaking tall oil pitch, extracting plant sterol of the present invention may further comprise the steps:
Step 1 added papermaking tall oil pitch, the pure and mild vitriol oil in the reactor drum, under stirring condition, is heated to 68 ℃～75 ℃, this temperature refluxed 2 hours;
Step 2 adds 70 ℃～80 ℃ hot water, leaves standstill and makes the pure and mild vitriol oil and material layering in 15～20 minutes, discards lower floor's water;
Step 3 contains the upper strata oil phase of plant sterol and fatty ester washes to neutral with 90 ℃～100 ℃ hot water, continues to be heated to 110 ℃～120 ℃;
Oil phase after step 4 will be washed separates fatty ester with the method for short-path distillation, when being specially short-path distillation, is fatty ester at 120 ℃～210 ℃ cuts, and the raffinate of staying behind the separating out fat acid esters in the still is the fluid that contains plant sterol;
Step 5 remains in the fluid that contains plant sterol in the still after having separated fatty ester, uses dissolution with solvents;
The plant sterol that step 6 is advanced dissolving in the solvent adsorbs through ion exchange resin, uses solvent elution after having adsorbed again;
After the step 7 solvent elution finishes, the solvent distillation is reclaimed, promptly get the article plant sterol that wets, wet article plant sterol passes through drying, pulverizes, and plant sterol gets product.
The method of from papermaking tall oil pitch, extracting plant sterol of the present invention; Alcohol described in the step 1 is methyl alcohol or ethanol; Add-on is 70%～100% of a raw material tall oil pitch weight, and the consumption of the vitriol oil described in the step 1 is 2%～4% of a raw material tall oil pitch weight, and the consumption of the water described in the step 2 is 20%～30% of a raw material tall oil pitch weight; Distillatory temperature described in the step 4 is 180 ℃～220 ℃; Distillatory vacuum tightness is 1～5Pa, and the solvent described in the step 5 is absolute ethyl alcohol, acetone, Virahol, and the ion exchange resin described in the step 6 is anionite-exchange resin; Solvent described in the step 6 is sherwood oil, normal hexane, butane, ETHYLE ACETATE, and the drying temperature described in the step 7 is 60 ℃～65 ℃.
The invention has the beneficial effects as follows: the present invention can directly extract plant sterol from the papermaking tall oil; And need from wood pulp, not extract tall oil, and then from tall oil, extract the step of plant sterol, compared with prior art; The plant sterol purity that the present invention has that raw materials cost is low, comprehensive utilization degree is high, extract is high, yield is high; Content reaches more than 99%, and yield reaches more than 80%, and trash discharge is few; Fatty acid ester that short-path distillation comes out and residue can be made tensio-active agent and Collophanite flotation collector respectively, help the characteristics of suitability for industrialized production and environmental protection.Simultaneously, because the raw material that this technology is selected for use is a paper pulp oil slick pitch, can significantly reduce the discharging of dirty oil in the paper industry, reduce the paper industry environmental pollution, therefore, this technology has great social benefit and economic benefit and vast potential for future development.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Below the present invention is described, but the present invention not merely is defined in these embodiment through specific embodiment.
Embodiment 1
The tall oil pitch, 45L methyl alcohol and the 0.55L vitriol oil that 50kg are contained 8.1% plant sterol add in the reaction kettle; Under stirring condition, be heated to 68 ℃; Refluxed then 2 hours, and added 100L75 ℃ hot water, left standstill 15 minutes; The water of lower floor's sulfur acid and methyl alcohol is discarded, keep the oil phase that the upper strata contains plant sterol and fatty ester.
Upper oil phase is washed to neutrality with 95 ℃ hot water, is heated to 110 ℃, and the moisture content in the oil phase is removed; The oil phase that will take off moisture content joins in the still kettle of short-path distillation, and vacuum tightness remains under the condition of 2Pa, and distillation temperature is 180 ℃; The fraction of collecting 120 ℃～210 ℃ is a fatty ester; The still raffinate that contains plant sterol in the evaporating kettle dissolves in the Virahol, through the absorption of anion-exchange resin, carries out wash-out with sherwood oil then again.
The sherwood oil that will contain plant sterol carries out solvent distillation and reclaims; Promptly get the wet article of plant sterol after having reclaimed sherwood oil; Wet article plant sterol is put in the baking oven 65 ℃ of freeze-day with constant temperature into and is pulverized through kibbler after 1.5 hours, promptly gets white finished product plant sterol 3.15kg; Sterol yield 80% is through gas chromatographic analysis sterol total content 99.05%.
Embodiment 2
The tall oil pitch, 45L methyl alcohol and the 1.0L vitriol oil that 50kg are contained 8.1% plant sterol add in the reaction kettle; Under stirring condition, be heated to 70 ℃; Refluxed then 2 hours, and added 100L70 ℃ hot water, left standstill 20 minutes; The water of lower floor's sulfur acid and methyl alcohol is discarded, keep the oil phase that the upper strata contains plant sterol and fatty ester.
Upper oil phase is washed to neutrality with 90 ℃ hot water, is heated to 115 ℃, and the moisture content in the oil phase is removed; The oil phase that will take off moisture content joins in the still kettle of short-path distillation, and vacuum tightness remains under the condition of 2Pa, and distillation temperature is 190 ℃; The fraction of collecting 120 ℃～210 ℃ is a fatty ester; The still raffinate that contains plant sterol in the evaporating kettle dissolves in the absolute ethyl alcohol, through the absorption of anion-exchange resin, carries out wash-out with normal hexane then again.
The sherwood oil that will contain plant sterol carries out solvent distillation and reclaims; Promptly get the wet article of plant sterol after having reclaimed sherwood oil; Wet article sterol is put in the baking oven 60 ℃ of freeze-day with constant temperature into and is pulverized through kibbler after 1.5 hours, promptly obtains white finished product plant sterol 3.32kg; Sterol yield 82% is through gas chromatographic analysis sterol total content 99.15%.
Embodiment 3
The tall oil pitch, 64L methyl alcohol and the 1.0L vitriol oil that 50kg are contained 8.1% plant sterol add in the reaction kettle; Under stirring condition, be heated to 72 ℃; Refluxed then 2 hours, and added 100L80 ℃ hot water, left standstill 18 minutes; The water of lower floor's sulfur acid and methyl alcohol is discarded, keep the oil phase that the upper strata contains plant sterol and fatty ester.
Upper oil phase is washed to neutrality with 98 ℃ hot water, is heated to 120 ℃, and the moisture content in the oil phase is removed; The oil phase that will take off moisture content joins in the still kettle of short-path distillation, and vacuum tightness remains under the condition of 2Pa, and distillation temperature is 195 ℃; The fraction of collecting 120 ℃～210 ℃ is a fatty ester; The still raffinate that contains plant sterol in the evaporating kettle dissolves in the acetone, through the absorption of anion-exchange resin, carries out wash-out with butane then again.
The sherwood oil that will contain plant sterol carries out solvent distillation and reclaims; Promptly get the wet article of plant sterol after having reclaimed sherwood oil; Wet article sterol is put in the baking oven 62 ℃ of freeze-day with constant temperature into and is pulverized through kibbler after 1.5 hours, promptly obtains white finished product plant sterol 3.43kg; Sterol yield 85% is through gas chromatographic analysis sterol total content 99.3%.
Embodiment 4
The tall oil pitch, 45L ethanol and the 0.55L vitriol oil that 50kg are contained 8.1% plant sterol add in the reaction kettle; Under stirring condition, be heated to 72 ℃; Refluxed then 2 hours, and added 100L80 ℃ hot water, left standstill 15 minutes; The water of lower floor's sulfur acid and methyl alcohol is discarded, keep the oil phase that the upper strata contains plant sterol and fatty ester.
Upper oil phase is washed to neutrality with 100 ℃ hot water, is heated to 120 ℃, and the moisture content in the oil phase is removed; The oil phase that will take off moisture content joins in the still kettle of short-path distillation, and vacuum tightness remains under the condition of 2Pa, and distillation temperature is 210 ℃; The fraction of collecting 120 ℃～210 ℃ is a fatty ester; The still raffinate that contains plant sterol in the evaporating kettle dissolves in the acetone, through the absorption of anion-exchange resin, carries out wash-out with ether then again.
The sherwood oil that will contain plant sterol carries out solvent distillation and reclaims; Promptly get the wet article of plant sterol after having reclaimed sherwood oil; Wet article sterol is put in the baking oven 65 ℃ of freeze-day with constant temperature into and is pulverized through kibbler after 1.5 hours, promptly obtains white finished product plant sterol 3.23kg; Sterol yield 80% is through gas chromatographic analysis sterol total content 99.1%.
Embodiment 5
The tall oil pitch, 45L ethanol and the 0.55L vitriol oil that 50kg are contained 8.1% plant sterol add in the reaction kettle; Under stirring condition, be heated to 75 ℃; Refluxed then 2 hours, and added 100L75 ℃ hot water, left standstill 15 minutes; The water of lower floor's sulfur acid and methyl alcohol is discarded, keep the oil phase that the upper strata contains plant sterol and fatty ester.
Upper oil phase is washed to neutrality with 95 ℃ hot water, is heated to 110 ℃, and the moisture content in the oil phase is removed; The oil phase that will take off moisture content joins in the still kettle of short-path distillation, and vacuum tightness remains under the condition of 2Pa, and distillation temperature is 220 ℃; The fraction of collecting 120 ℃～210 ℃ is a fatty ester; The still raffinate that contains plant sterol in the evaporating kettle dissolves in the Virahol, through the absorption of anion-exchange resin, carries out wash-out with ETHYLE ACETATE then again.
The sherwood oil that will contain plant sterol carries out solvent distillation and reclaims; Promptly get the wet article of plant sterol after having reclaimed sherwood oil; Wet article sterol is put in the baking oven 65 ℃ of freeze-day with constant temperature into and is pulverized through kibbler after 1.5 hours, promptly obtains white finished product plant sterol 3.28kg; Sterol yield 81% is through gas chromatographic analysis sterol total content 99.15%.
Claims (5)
1. method from papermaking tall oil bitumen extraction plant sterol may further comprise the steps:
Step 1: papermaking tall oil pitch, the pure and mild vitriol oil are added in the reactor drum, under stirring condition, be heated to 68 ℃～75 ℃, refluxed then 2 hours;
Step 2: add 70 ℃～80 ℃ hot water, left standstill 15～20 minutes, make the pure and mild vitriol oil and material layering, discard lower floor's water;
Step 3: the oil phase that the upper strata is contained plant sterol and fatty ester is extremely neutral with 90 ℃～100 ℃ hot water washing, continues to be heated to 110 ℃～120 ℃;
Step 4: the oil phase after will washing separates fatty ester with the method for short-path distillation, when being specially short-path distillation, is fatty ester at 120 ℃～210 ℃ cuts, and the raffinate of staying behind the separating out fat acid esters in the still is the fluid that contains plant sterol;
Step 5: remain in the oil plant that contains plant sterol in the still after having separated fatty ester, use dissolution with solvents;
Step 6: the plant sterol that advances dissolving in the solvent adsorbs through ion exchange resin, uses solvent elution after having adsorbed again;
Step 7: after solvent elution finishes, the solvent distillation is reclaimed, promptly get the article plant sterol that wets, wet article plant sterol passes through drying, pulverizes, and plant sterol gets product;
Wherein, the distillatory temperature described in the step 4 is 180～220 ℃, and distillatory vacuum tightness is 1～5Pa; Solvent described in the step 5 is absolute ethyl alcohol, acetone, Virahol; Ion exchange resin described in the step 6 is anionite-exchange resin, and the solvent described in the step 6 is sherwood oil, normal hexane, butane, ETHYLE ACETATE.
2. the method from papermaking tall oil bitumen extraction plant sterol according to claim 1; It is characterized in that: the alcohol described in the step 1 is methyl alcohol or ethanol; Add-on is 70%～100% of a raw material papermaking tall oil pitch weight, and the consumption of the vitriol oil described in the step 1 is 2%～4% of a raw material tall oil pitch weight.
3. the method from papermaking tall oil bitumen extraction plant sterol according to claim 1 is characterized in that: the consumption of the water described in the step 2 is 20%～30% of a raw material papermaking tall oil pitch weight.
4. the method from papermaking tall oil bitumen extraction plant sterol according to claim 1 is characterized in that: the drying temperature described in the step 7 is 60～65 ℃.
5. the method from papermaking tall oil bitumen extraction plant sterol according to claim 1 is characterized in that: may further comprise the steps:
Step 1 adds the pure and mild 1.0L vitriol oil of tall oil pitch, 64L that 50kg contains 8.1% plant sterol in the reaction kettle, under stirring condition, is heated to 68 ℃～75 ℃, refluxes then 2 hours;
Step 2 adds 100L75 ℃ hot water, leaves standstill 15 minutes, and the water of lower floor's sulfur acid with alcohol discarded, and keeps the oil phase that the upper strata contains plant sterol and fatty ester;
Step 3 is washed upper oil phase to neutrality with 95 ℃ hot water, continues to be heated to 110 ℃;
Step 4 removes the moisture content in the oil phase, and the oil phase that will take off moisture content joins in the still kettle of short-path distillation, and vacuum tightness remains under the condition of 2Pa, and distillation temperature is 180 ℃～220 ℃, and the fraction of collecting 120 ℃～210 ℃ is a fatty ester;
Step 5 is dissolved the still raffinate that contains plant sterol in the evaporating kettle with Virahol;
Step 6 is advanced the absorption of plant sterol through anion-exchange resin in the Virahol to dissolving, carries out wash-out with sherwood oil then;
The sherwood oil that step 7 will contain plant sterol distills; Reclaim sherwood oil distillation, has reclaimed and promptly got the plant sterol article that wet behind the sherwood oil, put in the baking oven plant sterol article that wet into 65 ℃ of freeze-day with constant temperature after 1.5 hours; Pulverize through kibbler, plant sterol gets product.
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| CN201010268028A CN101942008B (en) | 2010-08-31 | 2010-08-31 | Process for extracting phytosterol from papermaking wood pulp oil slick pitch |
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| CN101942008B true CN101942008B (en) | 2012-10-03 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102703104B (en) * | 2012-06-21 | 2013-12-04 | 遇秉武 | Production method for low-QI (Quality Index) coal pitch |
| CN104817962B (en) * | 2015-04-07 | 2017-03-29 | 怀化市双阳林化有限公司 | A kind of oily lignin separation method |
| CN105037473B (en) * | 2015-07-20 | 2017-11-03 | 宜春大海龟生命科学有限公司 | A kind of method of the purification sterol from tall oil |
| CN107417759B (en) * | 2017-08-11 | 2020-04-17 | 内蒙古昶辉生物科技股份有限公司 | Preparation method for extracting phytosterol and sterol ester from paper pulp oil slick asphalt |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1807444A (en) * | 2006-02-07 | 2006-07-26 | 南京工业大学 | Method for extracting plant sterol from plant oil asphalt |
| CN101412745A (en) * | 2008-11-27 | 2009-04-22 | 南京工业大学 | Improved process for extracting sterol from vegetable oil asphalt |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1807444A (en) * | 2006-02-07 | 2006-07-26 | 南京工业大学 | Method for extracting plant sterol from plant oil asphalt |
| CN101412745A (en) * | 2008-11-27 | 2009-04-22 | 南京工业大学 | Improved process for extracting sterol from vegetable oil asphalt |
Non-Patent Citations (1)
| Title |
|---|
| 李春荣等.由植物油沥青或塔尔油沥青中提取植物甾醇的工艺研究.《食品工业科技》.2004,第25卷(第6期),111-112. * |
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