CN103333751B - Method of producing powdered soap by using vegetable oil alkali refining nigre containing phospholipid - Google Patents
Method of producing powdered soap by using vegetable oil alkali refining nigre containing phospholipid Download PDFInfo
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- CN103333751B CN103333751B CN201210520123.9A CN201210520123A CN103333751B CN 103333751 B CN103333751 B CN 103333751B CN 201210520123 A CN201210520123 A CN 201210520123A CN 103333751 B CN103333751 B CN 103333751B
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Abstract
The invention relates to a method of producing powdered soap by using vegetable oil alkali refining nigre containing phospholipid. The method comprises a step of mixing and stirring the vegetable oil alkali refining nigre with hydrochloric acid for acidification, and separating a water phase, an emulsification phase and an oil phase after the mixture is layered; a step of mixing the emulsification phase with an organic solvent and extracting to obtain a phospholipid mixture; a step of adding lactic acid or acetic acid into the phospholipid mixture obtained after extraction that is performed to remove oil, adding hydrogen peroxide, and mixing, stirring and performing a hydroxylation reaction at 40-70 DEG C; a step of adding excess sodium hydroxide into the product of the hydroxylation reaction after the hydroxylation reaction is finished, and mixing, stirring and performing a saponification reaction at 50 DEG C; and a step of mixing the product of the saponification reaction with corn starch, and performing spray drying to obtain the powdered soap. According to the method provided by the invention, nigre produced by vegetable oil alkali refining can be made full use of, phospholipid contained in the nigre can be effectively recycled, and therefore problems of material waste and environmental pollution, which are caused by inadequate utilization of the vegetable oil alkali refining nigre, are prevented.
Description
Technical field
The present invention relates to a kind of utilization and containing the vegetable oil alkali refining soap stock of phosphatide, produce the method for soap powder, belong to vegetable oil production technical field.
Background technology
Oil plant obtains crude oil through squeezing or after leaching, and contains the compositions such as phosphatide, lipid acid in crude oil, needs refining to remove.By aquation, can remove most of hydrated phospholipid, not removed hydrated phospholipid, nonhydratable phosphatide, lipid acid, conventionally with adding sodium hydroxide alkali refining, obtain soap stock and alkali refining oil.When containing the soybean oil of phosphatide, rapeseed oil, the depickling of peanut wet goods oil alkali refining, can produce the soap stock that contains phosphatide.These vegetable oil alkali refining soap stocks account for the 4-5% of refining oil weight, and its main component is soda soap (20-35%), glyceryl ester (15-32%), phosphatide (5-20%), water (40-50%) and other impurity etc.1300 tons of/day current soybean oil production line for refining of San Hehuifu grain and oil group of take are example, produce the soap stock of 40 tons of left and right every day.Comprehensive utilization soap stock resource, not only can alleviate the pressure of sewage disposal, and can also increase the output value, increases economic efficiency.
At present, using the production technique of vegetable oil alkali refining soap stock is both at home and abroad generally soap stock to be produced to lipid acid with sulfuric acid acidation go forward side by side after a ground beetle esterification and prepare biofuel.The disclosed technical schemes such as CN102618388A, CN101338216A, CN101565654A, CN1970693A, CN101191065A, CN1931961A, CN100398629C, CN1916141A, CN1950491A be all in vegetable oil alkali refining soap stock soda soap and neutral fat utilize technology.Application number is the preparation method that 03112493.3 Chinese patent application discloses a kind of soap powder by using oil residue, it is with after dilute sulphuric acid acidifying by soybean oil residue, first use caustic soda saponification, add again sherwood oil, polyacrylamide and sodium laurylsulfonate to continue saponification, saponification resultant is with after hydrogen peroxide decolouring, add sodium carbonate and sodium laurylsulfonate and oleic acid single ethanol amide base succinic monoester salt mixed aid and mix after carry out the dry soap powder of making of spray dried.Above technical scheme is all the optimization process for sodium soap, to the phosphatide in soap stock, be all to process by strong acid and strong base, even and phosphatide is also difficult to hydrolysis under strong acid and strong base, therefore can produce a large amount of waste residues that is rich in phosphatide, for vegetable oil alkali refining soap stock, do not realize fully and utilizing like this, both wasted raw material, contaminate environment again, and there is not yet so far Patents technology and research report for the utilization of the phosphatide in vegetable oil alkali refining soap stock.
Summary of the invention
For solving the problems of the technologies described above, the object of the present invention is to provide a kind of production method of soap powder, by take, containing the vegetable oil alkali refining soap stock of phosphatide, as raw material, produce soap powder, realize the utilization for the phosphatide in vegetable oil alkali refining soap stock.
For achieving the above object, the invention provides a kind of utilization and containing the vegetable oil alkali refining soap stock of phosphatide, produce the method for soap powder, adopt hydrochloric acid to carry out acidifying to vegetable oil alkali refining soap stock, after stratification, isolate oil phase, Emulsion Phase and water; Then adopt oil phase substance remaining in the organic solvent extraction Emulsion Phases such as dehydrated alcohol, hexane to obtain and take phospholipid as main compound, then add hydrogen peroxide, acetic acid (or lactic acid) to carry out after hydroxylating, add sodium hydroxide to supplement saponification, then compound with raw materials such as W-Gums, make soap powder product after spray-dried.The method can comprise following concrete steps:
The mixed in hydrochloric acid that is 15-36wt% by vegetable oil alkali refining soap stock and concentration, regulating the pH value of mixture is 1-3, stirs acidifying 30-60 minute at 40-70 ℃, then standing 1-8 hour, isolates water, Emulsion Phase and oil phase after layering;
According to 1: 1-1: 5 volume ratio is mixed Emulsion Phase for the first time and extracted with organic solvent, separated single extraction liquid is afterwards again according to 1: 1-1: 5 volume ratio is mixed Emulsion Phase to carry out reextraction with organic solvent, obtains mixture of phospholipids and extraction fluid;
In the mixture of phospholipids extracting after oil removing, add lactic acid or the acetic acid that accounts for mixture of phospholipids weight 3-10%, add again the hydrogen peroxide that accounts for described mixture of phospholipids weight 10-20%, in 40-70 ℃ of mix and blend 1-3 hour, carry out hydroxylating, wherein, the concentration of lactic acid or acetic acid is 30-75wt%, and the concentration of hydrogen peroxide is 10-30wt%;
After hydroxylating finishes, in the product of hydroxylating, add excessive sodium hydroxide, in 50 ℃ of mix and blend 1-3 hour, carry out saponification reaction;
The product of saponification reaction is mixed with the W-Gum that accounts for its weight 3-9%, then water is adjusted into 10-40wt% (in the total amount of product and the W-Gum of saponification reaction) by mixture concentration, then at 90-180 ℃, sprays dry, obtain soap powder.
In aforesaid method provided by the present invention, the oil phase that separation obtains can obtain stearic acid through cracking, hydrogenation, therefore, preferably, aforesaid method can also comprise processes the stearic step of preparation to oil phase, that is: oil phase is mixed with the water that accounts for its quality 10-50%, under the condition of 1-6MPa, 180-275 ℃, react 10 minutes to 1 hour, after separation of fatty acids, again under 180-210 ℃, the condition of 2-3MPa, nickel catalyzator, pass into hydrogen reaction 1-3 hour, prepare stearic acid.More preferably, the consumption of above-mentioned nickel catalyzator may be controlled to the 0.1-0.3wt% of the oil phase gross weight after separation of fatty acids.
According to specific embodiment of the invention scheme, preferably, aforesaid method is further comprising the steps of: stearic acid is mixed with the product of hydroxylating, then carry out together saponification reaction, that is: after hydroxylating finishes, after the stearic acid that the product of hydroxylating is prepared with oil phase mixes, add excessive sodium hydroxide, in 50 ℃ of mix and blend 1-3 hour, carry out saponification reaction.
According to specific embodiment of the invention scheme, preferably, the organic solvent that aforesaid method adopts is dehydrated alcohol or normal hexane etc.
According to specific embodiment of the invention scheme, preferably, aforesaid method can also comprise the step that reclaims solvent, that is: single extraction liquid and extraction fluid are mixed, and obtains hybrid extraction liquid; At-0.080MPa, to the temperature condition of the vacuum tightness of-0.0094MPa, 50-70 ℃, hybrid extraction liquid is carried out to distillating recovering solvent, the recycle after rectifying of resulting ethanol, resulting normal hexane divides recycle after water.
According to specific embodiment of the invention scheme, preferably, aforesaid method is further comprising the steps of: water is neutralized, then prepare sodium-chlor.
The method that utilization provided by the present invention is produced soap powder containing the vegetable oil alkali refining soap stock of phosphatide can be carried out according to the flow process shown in Fig. 1, and it can carry out according to following concrete steps:
(1) vegetable oil alkali refining soap stock is added in stirred tank, adding concentration is the hydrochloric acid of 15-36wt%, and regulating the pH value of mixture is 1-3, under 40-70 ℃ of condition of normal pressure, stirs acidifying 30-60 minute, then standing 1-8 hour isolates respectively water, Emulsion Phase and oil phase after layering;
(2) oil phase is inputted in reactor, the water that adds the 10-50% that accounts for oil phase weight, under the condition of 1-6MPa, 180-275 ℃, react 10 minutes to 1 hour, after separation of fatty acids, again under 180-210 ℃, the condition of 2-3MPa, 0.1-0.3% nickel catalyzator (consumption is in reaction-ure mixture), pass into hydrogen reaction 1-3 hour, prepare stearic acid; The water that separation obtains is through preparing sodium-chlor after neutralization;
(3) Emulsion Phase is delivered in extractor, according to the water content of Emulsion Phase, again by Emulsion Phase: organic solvent (dehydrated alcohol or normal hexane)=1: 1-1: 5 volume ratio adds organic solvent (dehydrated alcohol or normal hexane) to carry out single extraction, obtains single extraction liquid; Again by Emulsion Phase: organic solvent (dehydrated alcohol or normal hexane)=1: 1-1: 5 volume ratio adds organic solvent (dehydrated alcohol or normal hexane) to carry out reextraction, obtain mixture of phospholipids, extraction fluid (ethanol phase or normal hexane phase) is mixed with single extraction liquid, obtain hybrid extraction liquid;
(4) hybrid extraction liquid is pumped in vaporizer by solvent pump, at-0.080MPa, to distillating recovering solvent under the temperature condition of the vacuum tightness of-0.0094MPa, 50-70 ℃, ethanol rectifying or hexane divide recycle after water;
(5) mixture of phospholipids after extraction oil removing is delivered in reactor, add lactic acid (concentration is 30-75wt%) and hydrogen peroxide (concentration is 10-30wt%) or acetic acid (concentration is 30-75wt%) and hydrogen peroxide (concentration is 10-30wt%), in 40-70 ℃ of mix and blend 1-3 hour, carry out hydroxylating;
(6) after hydroxylating finishes, the product of hydroxylating is mixed with stearic acid, directly in reactor, add excessive sodium hydroxide, in 50 ℃ of mix and blend 1-3 hour, carry out saponification reaction;
(7) by the product of saponification reaction with to account for the W-Gum of its weight 3-9% composite, then water to adjust mixture concentration be 10-40wt%, be delivered to spray drying device, under the condition of 90-180 ℃, the dry soap powder product that obtains of spraying.
The present invention also provides a kind of soap powder, and it is to be prepared by above-mentioned method.
Aforementioned production method utilization provided by the invention is raw material production soap powder containing the vegetable oil alkali refining soap stock of phosphatide, can make full use of the soap stock producing after vegetable oil alkali refining, phosphatide in efficient recovery soap stock, avoids lacking for vegetable oil alkali refining soap stock wastage of material and the problem of environmental pollution that makes full use of and cause.The raw material of the soap powder product that the present invention produces, mainly from plant material, can all be recycled Emulsion Phase, and after laundry decontamination, in environment, easily degraded, is the washing composition of environmental protection.
Accompanying drawing explanation
Fig. 1 is that the schematic flow sheet of the method for soap powder is produced in utilization provided by the invention containing the vegetable oil alkali refining soap stock of phosphatide.Embodiment
For technical characterictic of the present invention, object and beneficial effect being had more clearly, understand, existing technical scheme of the present invention is carried out to following detailed description, but can not be interpreted as restriction that can practical range of the present invention.
Embodiment 1
The present embodiment provides a kind of utilization containing the vegetable oil alkali refining soap stock of phosphatide, to produce the method for soap powder, and its idiographic flow as shown in Figure 1.The method comprises the following steps:
Vegetable oil alkali refining soap stock is added in stirred tank, and adding concentration is 36% concentrated hydrochloric acid, regulates soap stock pH to 1, under 50 ℃, condition of normal pressure, stirs acidifying 30 minutes; Then after standing 4 little layereds, isolate respectively water, Emulsion Phase and oil phase;
Oil phase is inputted in reactor, add again the water that accounts for oil phase weight 10%, under 5MPa, the condition of 263 ℃, react 10 minutes, triglyceride level in cracking oil phase generates lipid acid, after separation of fatty acids, again under 200 ℃, the condition of 2MPa, 0.1% nickel catalyzator, pass into hydrogen reaction and within 1 hour, carry out deep hydrogenation and prepare stearic acid;
The water that separation obtains is through preparing sodium-chlor after neutralization;
Emulsion Phase is delivered in extractor, according to Emulsion Phase: dehydrated alcohol=1: 3 volume ratio adds dehydrated alcohol to carry out single extraction, isolates single extraction liquid; And then according to Emulsion Phase: dehydrated alcohol=1: 1 volume ratio adds dehydrated alcohol to carry out reextraction to obtain mixture of phospholipids and extraction fluid (dehydrated alcohol phase), single extraction liquid and extraction fluid are merged, obtain hybrid extraction liquid; Hybrid extraction liquid after merging is pumped in vaporizer by solvent pump, and Distillation recovery ethanol under the-vacuum tightness of 0.0094MPa, the temperature condition of 60 ℃, obtains dehydrated alcohol after rectifying;
Mixture of phospholipids after extraction oil removing is delivered in reactor, adds the acetic acid (concentration is 55wt%) and 30% hydrogen peroxide (concentration is 20wt%) that account for mixture of phospholipids quality 10%, in 40 ℃ of mix and blends, within 3 hours, carry out hydroxylating;
After hydroxylating finishes, directly to the stearic acid that adds hydrogenation to obtain in reactor, then add excessive sodium hydroxide, in 50 ℃ of mix and blends, within 1 hour, carry out saponification reaction;
After saponification reaction finishes, by the product of saponification reaction with to account for the W-Gum of its quality 6% compound, then water to adjust mixture concentration be 15wt%, be delivered to spray drying device, under the condition of 100 ℃, spraying is dry obtains faint yellow soap powder product.
According to the light industry standard QB/T2387-2008 < < of the People's Republic of China (PRC) laundry powdered soap > > detection method of the National Development and Reform Commission of People's Republic of China (PRC) issue, the soap powder of embodiment 1 preparation is detected, record index as follows: pH (0.1% solution, 25 ℃) be 10, free alkali content is 3.1%, and apparent density is 0.34g/cm
3, dry soda soap content is 42%, and gross activity substances content is 45%, and moisture content and volatile content are 6%; Soil removability II level; The pH that its indices is better than stipulating in standard (0.1% solution, 25 ℃)≤10.5, free alkali≤8%, apparent density>=0.3g/cm
3, dry soda soap>=7%, gross activity material>=13%, the standard of moisture content and volatile matter≤15%.
Embodiment 2
The present embodiment provides a kind of utilization containing the vegetable oil alkali refining soap stock of phosphatide, to produce the method for soap powder, and its idiographic flow as shown in Figure 1.The method comprises the following steps:
Vegetable oil alkali refining soap stock is added in stirred tank, and adding concentration is the concentrated hydrochloric acid of 15wt%, regulates soap stock pH to 3, under 70 ℃, condition of normal pressure, stirs acidifying 60 minutes, then, after standing 8 little layereds, isolates respectively water, Emulsion Phase and oil phase;
Oil phase is inputted in reactor, add again the water that accounts for oil phase quality 10%, under 1MPa, the condition of 180 ℃, react 60 minutes, triglyceride level in cracking oil phase generates lipid acid, after separation of fatty acids, again under 100 ℃, the condition of 2MPa, 0.3% nickel catalyzator, pass into hydrogen reaction and within 3 hours, carry out deep hydrogenation and prepare stearic acid;
The water that separation obtains is through preparing sodium-chlor after neutralization;
Emulsion Phase is delivered in extractor, according to Emulsion Phase: normal hexane=1: 5 volume ratio adds normal hexane to carry out single extraction, isolates single extraction liquid; Then according to Emulsion Phase: normal hexane=1: 1 volume ratio adds normal hexane to carry out reextraction to obtain mixture of phospholipids and extraction fluid (hexane phase), single extraction liquid and extraction fluid are merged, obtain hybrid extraction liquid; Hybrid extraction liquid is pumped in vaporizer by solvent pump, Distillation recovery hexane under the-vacuum tightness of 0.0080MPa, the temperature condition of 50 ℃, evaporation concentration liquid can merge with oil phase;
Mixture of phospholipids after extraction oil removing is delivered in reactor, add the lactic acid (concentration is 75%) that accounts for mixture of phospholipids quality 4% and the hydrogen peroxide (concentration is 30%) that accounts for mixture of phospholipids quality 20%, in 70 ℃ of mix and blends, within 1 hour, carry out hydroxylating;
After hydroxylating finishes, directly in reactor, add excessive sodium hydroxide, the stearic acid that adds hydrogenation to obtain, carries out saponification reaction for 1 hour in 70 ℃ of mix and blends;
After saponification reaction finishes, by saponification resultant with to account for the W-Gum of its quality 9% compound, then water to adjust mixture concentration be 15%, be delivered to spray drying device, under the condition of 180 ℃, spraying obtains faint yellow soap powder product after dry.
According to the light industry standard QB/T2387-2008 < < of the People's Republic of China (PRC) laundry powdered soap > > detection method of the National Development and Reform Commission of People's Republic of China (PRC) issue, the soap powder of embodiment 2 preparations is detected, record index as follows: pH (0.1% solution, 25 ℃) be 10, free alkali content is 3%, and apparent density is 0.32g/cm
3, dry soda soap content is 38%, and gross activity substances content is 40%, and moisture content and volatile content are 3.3%; Soil removability II level; The pH that its index is better than stipulating in standard (0.1% solution, 25 ℃)≤10.5, free alkali≤8%, apparent density>=0.3g/cm
3, dry soda soap>=7%, gross activity material>=13%, the standard of moisture content and volatile matter≤15%.
Claims (6)
1. a method for soap powder is produced in utilization containing the vegetable oil alkali refining soap stock of phosphatide, and it comprises the following steps:
The mixed in hydrochloric acid that is 15-36wt% by vegetable oil alkali refining soap stock and concentration, regulating the pH value of mixture is 1-3, stirs acidifying 30-60 minute at 40-70 ℃, then standing 1-8 hour, isolates water, Emulsion Phase and oil phase after layering;
Volume ratio according to 1:1-1:5 is mixed Emulsion Phase for the first time and is extracted with organic solvent, after separated single extraction liquid, according to the volume ratio of 1:1-1:5, Emulsion Phase is mixed and carries out reextraction with organic solvent again, obtain mixture of phospholipids and extraction fluid;
To extracting in the mixture of phospholipids obtaining after oil removing, add lactic acid or the acetic acid that accounts for described mixture of phospholipids weight 3-10%, add again the hydrogen peroxide that accounts for described mixture of phospholipids weight 10-20%, in 40-70 ℃ of mix and blend 1-3 hour, carry out hydroxylating, wherein, the concentration of lactic acid or acetic acid is 30-75wt%, and the concentration of hydrogen peroxide is 10-30wt%;
Oil phase is mixed with the water that accounts for its quality 10-50%, under the condition of 1-6MPa, 180-275 ℃, react 10 minutes to 1 hour, after separation of fatty acids, then under 180-210 ℃, the condition of 2-3MPa, nickel catalyzator, pass into hydrogen reaction 1-3 hour, prepare stearic acid;
Described stearic acid is mixed with the product of hydroxylating, add excessive sodium hydroxide, in 50 ℃ of mix and blend 1-3 hour, carry out saponification reaction;
After the product of saponification reaction is mixed with the W-Gum that accounts for its weight 3-9%, then water is adjusted into 10-40wt% by mixture concentration, then at 90-180 ℃, sprays dry, obtains soap powder.
2. method according to claim 1, wherein, the consumption of described nickel catalyzator is controlled the 0.1-0.3wt% for the oil phase gross weight after separation of fatty acids.
3. method according to claim 1, wherein, described organic solvent is dehydrated alcohol or normal hexane.
4. method according to claim 3, it is further comprising the steps of: single extraction liquid and extraction fluid are mixed, obtain hybrid extraction liquid;
At-0.080MPa, to the temperature condition of the vacuum tightness of-0.0094MPa, 50-70 ℃, hybrid extraction liquid is carried out to distillating recovering solvent, the recycle after rectifying of resulting ethanol, resulting normal hexane divides recycle after water.
5. method according to claim 1, it is further comprising the steps of: water is neutralized, then prepare sodium-chlor.
6. a soap powder, it is prepared by the method for producing soap powder containing the vegetable oil alkali refining soap stock of phosphatide by the utilization described in claim 1-5 any one.
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| CN103571981B (en) * | 2013-10-28 | 2015-04-22 | 浙江理工大学 | Preparation method of antibacterial and antifungal fat-liquoring agent suitable for aged leather |
| CN106046916A (en) * | 2016-08-09 | 2016-10-26 | 丁玉琴 | Preparation method of gel pen ink cleanser |
| CN109971548B (en) * | 2017-12-27 | 2023-08-08 | 丰益(上海)生物技术研发中心有限公司 | Preparation method of nigre and fatty acid calcium |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102018156A (en) * | 2009-09-15 | 2011-04-20 | 广州市食品工业研究所有限公司 | Method of synthesizing phosphatide emulsifier for food |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102018156A (en) * | 2009-09-15 | 2011-04-20 | 广州市食品工业研究所有限公司 | Method of synthesizing phosphatide emulsifier for food |
Non-Patent Citations (1)
| Title |
|---|
| 赵海伶.菜籽油脚中磷脂的研究.《中国优秀博硕士学位论文全文数据库（硕士）工程科技I辑》.2004, * |
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