CN103666772A - Polyoxyethylene sorbitan fatty acid ester prepared by use of waste oil - Google Patents
Polyoxyethylene sorbitan fatty acid ester prepared by use of waste oil Download PDFInfo
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- CN103666772A CN103666772A CN201210355426.XA CN201210355426A CN103666772A CN 103666772 A CN103666772 A CN 103666772A CN 201210355426 A CN201210355426 A CN 201210355426A CN 103666772 A CN103666772 A CN 103666772A
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- fatty acid
- acid ester
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Abstract
The invention discloses polyoxyethylene sorbitan fatty acid ester prepared by use of waste oil, which is prepared by the following steps: preparing sorbitan fatty acid ester by use of waste oil; introducing ethylene oxide into the waste oil sorbitan fatty acid ester; and adding a catalyst lithium hydroxide and controlling the temperature at 100-160 DEG C and the time at 2 hours to obtain the waste oil polyoxyethylene sorbitan fatty acid ester. In the invention, the adopted equipment is a reaction kettle of a stainless steel (or enamel) material; and the reaction kettle is provided with devices for closing, pressurization, pressure reduction, heating, cooling, ethylene oxide introduction and the like. The polyoxyethylene sorbitan fatty acid ester disclosed by the invention is light brown waxy solid, is soluble to water with little toxicity, and causes low irritation to the skin and mucosa of a human body; and the acid value (mgKOH/g) is lower than or equal to 8, the saponification value (mgKOH/g) is 75-95, the water content is less than or equal to 1.0%, and the pH value is 6-8. The polyoxyethylene sorbitan fatty acid ester disclosed by the invention is a recyclable new material in modern environmental protection and has great social and economic benefits.
Description
[technical field]
The present invention utilizes abendoned oil to manufacture fatty acid loss water sorbit ester Soxylat A 25-7.The present invention is hydrophilic emulsifier, solubilizing agent, softening agent, is good fiber lubricant.
[background technology]
The present invention can be used for machine oil cleaning additive, the emulsifying agent of coating, chemical industry, petroleum drilling weighted mud emulsifying agent; In paint, coatings industry, do dispersion agent, in pesticide producing, do wetting agent, emulsifying agent; In petroleum product, make solubility promoter, in weaving and leather, do lubricant and softening agent, for O/W type polyamide fibre and viscose glue tyre cord oiling agent, fiber is had to good smoothing effect and also can make the rust-preventive agent of slushing oil.
The present invention is the novel material of modern environment protection reproducible utilization, has good Social benefit and economic benefit.
[summary of the invention]
The present invention utilizes refining crude oil and the pre-esterification of methyl alcohol of abendoned oil, adds an acidic catalyst 0.5-1.0%, working pressure 0.4-0.6kg/cm in still
2, temperature is controlled at 65-85 ℃, 1 hour time.Control the acid value≤3.5mgKOH/g of refining crude oil.
After the refining pre-esterification of crude oil of abendoned oil of the present invention, under the condition of basic catalyst, carry out formal esterification having.Method: adding basic catalyst 0.3-0.9%, abendoned oil and methyl alcohol molar ratio is 1: 4-1: 9, temperature is controlled 60-80 ℃, 1 hour methanol eddy reaction times.Obtain waste grease fatty acid methyl esters and glycerine, separated waste grease fatty acid methyl esters and glycerine, then wash, distill, obtain refining waste grease fatty acid methyl esters and glycerine.
Abendoned oil methyl esters treating process of the present invention: washing, charcoal absorption, filter filter, vacuum distilling, stand-by.
Anhydrous sorbitol making method: sorbyl alcohol is done under catalyzer, 140 degrees celsius at a small amount of sulfuric acid, stirring, vacuum hydro-extraction generate Isosorbide-5-Nitrae-anhydrous sorbitol or 1,4,3,6-, bis-anhydrous sorbitols, concrete which kind of product that generates, depends on Heating temperature and lasting time of reaction.
The refining waste grease fatty acid methyl esters of the present invention and Isosorbide-5-Nitrae-mistake anhydrous sorbitol carry out transesterify, synthesize the sour sorbitan ester of abendoned oil fat.Calculate abendoned oil methyl esters and anhydrous sorbitol reaction mol ratio and weight, add respectively in reactor, add under basic catalyst potassium hydroxide 0.5-1%, 80-100 ℃ of temperature control, vacuum state and react after 1.5-2 hour, synthesize the sour sorbitan ester of abendoned oil fat.
Equipment used of the present invention is the reactor of stainless steel (or enamel) material, and that this reactor has is airtight, pressurize, reduce pressure, heat, lower the temperature and have oxyethane the device such as to pass into.
The present invention utilizes abendoned oil to manufacture after the sour sorbitan ester of abendoned oil fat, calculate the abendoned oil sour sorbitan ester of fat and the oxyethane chemical reaction mole when actual weight that drops into, the sour sorbitan ester of abendoned oil fat is passed into oxyethane, add basic catalyst lithium hydroxide 0.5-1%, 100-160 ℃ of temperature control, time to control 2 hours, manufacture the sour sorbitan ester Soxylat A 25-7 of abendoned oil fat.
Outward appearance of the present invention is light brown oily body, water-soluble, acid value (mgKOH/g)≤8, saponification value (mgKOH/g) 75～95, moisture≤1.0%, pH value 6-8, to human body skin and mucous membrane nonirritant.
[embodiment]
Waste grease of the present invention, through physics, chemical pre-treatment, carries out its abendoned oil fat acid of gc analysis and forms: stearic acid (containing unsaturated hydrocarbons) 74-75%, palmitic acid (containing unsaturated hydrocarbons) 13-14%, other lipid acid 11-13%.
The first step of the present invention, the refining crude oil of abendoned oil and the pre-esterification of methyl alcohol.1000 kilograms of metering abendoned oils, heat up 40 ± 5 ℃, and 80 kilograms of metering methyl alcohol, add an acidic catalyst 0.5%, working pressure 0.4kg/cm in still
2, temperature is controlled at 75 ± 5 ℃, 1 hour reaction times.Control the acid value≤3.5mgKOH/g of refining crude oil.
Second step of the present invention, after the refining pre-esterification of crude oil of abendoned oil, carries out formal esterification having under the condition of basic catalyst.
Method: measure 300 kilograms of methyl alcohol and add in 16 kilograms of input reactors of basic catalyst, temperature heats up, control 70 ± 5 ℃, 1 hour methanol eddy reaction times, obtain waste grease fatty acid methyl esters and glycerine, after static 20 minutes, separated waste grease fatty acid methyl esters and glycerine, then by washing, distillation, obtain refining waste grease fatty acid methyl esters.
The present invention's the 3rd step, abendoned oil methyl esters is refining: washing, charcoal absorption, filter filter, vacuum distilling, through this four step, process, and the high boiling material in methyl esters, pigment, impurity can well be removed.
1. washing: temperature is controlled at 70 ± 5 ℃, stirs 20 minutes,
2. charcoal absorption: temperature is controlled at 70 ± 5 ℃, stirs 20 minutes.
3. filter filters: charcoal absorption methyl esters material enters filter, and it is stand-by that the methyl esters after filtration enters another storage tank.
4. vacuum distilling: add 1/2nd of whole methyl esters material, distill after 1-2 hour, lower the temperature 50 ± 5 ℃, then add second half methyl esters material.While seeing without effluent in observing visor, prove methyl ester distilled complete.Distillation vacuum degree control: 700-760mmHg, distillation temperature is controlled: 150-250 ℃.When temperature of reaction kettle is down to 100 ± 5 ℃, close vacuum.Refining methyl esters yield 94-97%.
The present invention's the 4th step, the sour sorbitan ester manufacture craft of the synthetic abendoned oil fat of transesterify of refining waste grease fatty acid methyl esters and anhydrous sorbitol:
Monoesters synthetic method:
Monoesters is synthetic is to calculate and feed intake with 1mol waste grease fatty acid methyl esters and 1mol sorbyl alcohol, and basic catalyst (NaHCO3) calculates with 0.8% of whole material.
1. measure 375 kilograms of sorbyl alcohols, be heated to 60 ± 5 ℃ of stirrings.
2. temperature rises to 110 ± 5 ℃ and carries out between sorbyl alcohol hydroxyl etherificate dehydration, and the time is controlled at 2.5 hours, and while measuring hydroxyl valency (mgKOH/g) 1150-1350, between sorbyl alcohol hydroxyl, etherificate is dehydrated into 1,4 anhydrous sorbitols.
3. measure 600 kilograms of abendoned oil methyl esters, with in vacuum pump sucting reaction still, stir.
4. measure 7.5 kilograms of basic catalysts, add in reactor, stir, open vacuum valve.
5. being warming up to 70 ± 5 ℃ has methyl alcohol to flow out, and reaches 110 ℃ to temperature, and methyl alcohol effluent stops substantially.Stop vacuum pump, reaction continues 2 hours, carries out material aging.
6. measure system acid value (mgKOH/g)≤8 o'clock, reaction terminating.
7. digestion time is complete, is cooled to rapidly 50 ± 5 ℃, discharging.
Three esters are synthetic is to calculate and feed intake with 3mol waste grease fatty acid methyl esters and 1mol sorbyl alcohol, and basic catalyst (NaHCO3) calculates with 0.8% of whole material.
1. measure 167 kilograms of sorbyl alcohols, be heated to 60 ± 5 ℃ of stirrings.
2. temperature rises to 110 ± 5 ℃ and carries out between sorbyl alcohol hydroxyl etherificate dehydration, and the time is controlled at 2.5 hours, and while measuring hydroxyl valency (mgKOH/g) 1150-1350, between sorbyl alcohol hydroxyl, etherificate is dehydrated into 1,4 anhydrous sorbitols.
3. measure 800 kilograms of abendoned oil methyl esters, with in vacuum pump sucting reaction still, stir.
4. measure 7.7 kilograms of basic catalysts, add in reactor, stir, open vacuum valve.
5. being warming up to 70 ± 5 ℃ has methyl alcohol to flow out, and reaches 110 ℃ to temperature, and methyl alcohol effluent stops substantially.Stop vacuum pump, reaction continues 2 hours, carries out material aging.
6. measure system acid value (mgKOH/g)≤8 o'clock, reaction terminating.
7. digestion time is complete, is cooled to rapidly 45 ± 5 ℃, discharging.
The present invention's the 5th step, the manufacture craft of the sour sorbitan ester Soxylat A 25-7 of abendoned oil fat:
310 kilograms of sour sorbitan esters of abendoned oil fat are added in people's reactor, and temperature is warming up to 40 ± 2 ℃ and starts to stir; Measure 10 kilogram of 50% lithium hydroxide aqueous solution (catalyzer), temperature is warming up to 105 ± 2 ℃ and starts decompression, stirring dehydration; After water takes off to the greatest extent, the air with in nitrogen replacement reactor, starts to pass into oxyethane, and oxyethane, when under meter measures to 800 kilograms, stops passing into, and the time is controlled 2 hours.Pass into oxyethane bulk temperature and be controlled at 150-160 ℃, pressure 0.2-0.3MPa.After passing into oxyethane and finishing, be cooled to 80 ± 2 ℃, add 7.5 kilograms of acetic acid to neutralize.Continue to stir dehydration, control moisture content≤1.0%, can stop dehydration.When temperature is down to normal temperature state, measure Specifications, qualified rear filtration packs packing into.
Waste water of the present invention needs after purifying treatment, can discharge.
Claims (6)
1. the present invention utilizes abendoned oil to manufacture fatty acid loss water sorbit ester Soxylat A 25-7.
2. according to claim 1, the present invention utilizes abendoned oil to manufacture fatty acid loss water sorbit ester Soxylat A 25-7.The present invention is that abendoned oil is manufactured after fatty acid loss water sorbit ester, the sour sorbitan ester of abendoned oil fat is passed into oxyethane, add catalyzer lithium hydroxide, temperature to be controlled at 100-160 ℃, time and be controlled at 2 hours, produce the sour sorbitan ester Soxylat A 25-7 of abendoned oil fat.
3. according to claim 1, equipment used of the present invention is the reactor of stainless steel (or enamel) material, and that this reactor has is airtight, pressurize, reduce pressure, heat, lower the temperature and have oxyethane the device such as to pass into.
4. light brown in appearance waxy solid of the present invention, water-soluble, very low toxicity,, acid value (mgKOH/g)≤8 very low to human body skin and mucous membrane irritation, saponification value (mgKOH/g) 75～95, moisture≤1.0%, pH value 6-8 according to claim 1.
5. according to claim 1, the present invention can be used for machine oil cleaning additive, the emulsifying agent of coating, chemical industry, petroleum drilling weighted mud emulsifying agent; In paint, coatings industry, do dispersion agent, in pesticide producing, do wetting agent, emulsifying agent; In petroleum product, make solubility promoter, in weaving and leather, do lubricant and softening agent, for O/W type polyamide fibre and viscose glue tyre cord oiling agent, fiber is had to good smoothing effect and also can make the rust-preventive agent of slushing oil.
6. according to claim 1, the present invention is the novel material of modern environment protection reproducible utilization, has good Social benefit and economic benefit.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210355426.XA CN103666772A (en) | 2012-09-24 | 2012-09-24 | Polyoxyethylene sorbitan fatty acid ester prepared by use of waste oil |
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| CN201210355426.XA CN103666772A (en) | 2012-09-24 | 2012-09-24 | Polyoxyethylene sorbitan fatty acid ester prepared by use of waste oil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104877833A (en) * | 2015-06-22 | 2015-09-02 | 天津博克尼科技发展有限公司 | Preparation method for automobile engine cleaning agent |
| CN107325274A (en) * | 2017-08-28 | 2017-11-07 | 辽宁奥克医药辅料股份有限公司 | A kind of preparation method of low color polyoxyethylene sorbitan monoleate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102030896A (en) * | 2010-11-15 | 2011-04-27 | 上海豪胜化工科技有限公司 | Polyalkylene oxide catalyst with medium-low molecular weight and preparation method thereof |
-
2012
- 2012-09-24 CN CN201210355426.XA patent/CN103666772A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030896A (en) * | 2010-11-15 | 2011-04-27 | 上海豪胜化工科技有限公司 | Polyalkylene oxide catalyst with medium-low molecular weight and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| 刘广文: "《农药水分散粒剂》", 31 January 2009, 化学工业出版社 * |
| 张贤丰等: "新型食品添加剂司盘和吐温", 《浙江化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104877833A (en) * | 2015-06-22 | 2015-09-02 | 天津博克尼科技发展有限公司 | Preparation method for automobile engine cleaning agent |
| CN107325274A (en) * | 2017-08-28 | 2017-11-07 | 辽宁奥克医药辅料股份有限公司 | A kind of preparation method of low color polyoxyethylene sorbitan monoleate |
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Application publication date: 20140326 |