CN104946404A - Production technology of stearic acid and oleic acid - Google Patents
Production technology of stearic acid and oleic acid Download PDFInfo
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- CN104946404A CN104946404A CN201510261271.7A CN201510261271A CN104946404A CN 104946404 A CN104946404 A CN 104946404A CN 201510261271 A CN201510261271 A CN 201510261271A CN 104946404 A CN104946404 A CN 104946404A
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- oleic acid
- stearic acid
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- dehydration
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/005—Splitting up mixtures of fatty acids into their constituents
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/02—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils
- C11C1/04—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils by hydrolysis
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
- C11C1/10—Refining by distillation
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
- C11C1/10—Refining by distillation
- C11C1/103—Refining by distillation after or with the addition of chemicals
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to a production technology of stearic acid and oleic acid. The production technology comprises the following steps: performing refining purification, hydrolysis, dehydration, primary squeezing, distillation, cooling and secondary squeezing; performing refining purification and then hydrolysis to obtain a mixed solution of stearic acid and oleic acid; after the hydrolysis, standing for separation; after the separation, dehydrating the oil layer and performing primary squeezing to remove stearic acid; separating to obtain crude oleic acid; distilling and cooling the crude oleic acid; and performing secondary squeezing to remove palmitic acid to obtain a finished product of oleic acid. According to the production technology of stearic acid and oleic acid, the technology is simple, the cost is relatively low, the separation of oleic acid and stearic acid is relatively thorough, and the product quality is stable.
Description
Technical field
The present invention relates to grease field of deep, be specifically related to the production technique of a kind of stearic acid and oleic acid.
Background technology
Stearic acid and oleic acid are all widely used at makeup, plastics, rubber materials, but the method ubiquity cost of current production stearic acid and oleic acid is high, unstable product quality, oleic acid is separated not thorough with stearic acid, cause there is stearic acid in oleic acid, there is oleic acid in stearic acid, cause the decline of the waste of raw material and the raising of cost and product quality.
Domestic stearic acid produce mainly with import plam oil for after raw material entered shortening, carrying out highly pressured hydrolysis, fatty acid, then carry out underpressure distillation system.But have a large amount of oleic acid in the stearic acid of finished product, the purity causing stearic acid product is like this not high, and wastes a large amount of oleic acid.Stearic raw material is palmitinic acid, and the inside is that be through hydrogenation and become stearic, most of situation is that hydrogenation does not thoroughly cause certainly containing C18:1.So almost having no way, is exactly that product iodine number is defective, two kinds for the treatment of methods, and when secondary material process or returning charge hydrogenation again, and palmitic hydrogenation process is loaded down with trivial details, comparatively complicated.
Summary of the invention
For solving the problem, the invention provides a kind of production technique simultaneously can producing stearic acid and oleic acid, technique is simple, and old lower, and oleic acid is separated comparatively thorough with stearic acid, constant product quality.
The technical solution adopted in the present invention
A production technique for stearic acid and oleic acid, comprises the following steps: refining purification, hydrolysis, dehydration, single pressing, distillation, cooling and twice pressing; Described hydrolysing step is: select animal-plant oil and emulsion to be stock oil, the mass ratio 100:3-5 of animal-plant oil and emulsion, stock oil, the 95-98% vitriol oil and quality are than being 100:[10-11]: [71-78], the temperature of reaction of controlled hydrolysis is 105-115 DEG C, the pressure of hydrolysis is at 63-68bar, and the time of hydrolysis is 2-2.5 hour; After hydrolysis, standing separatory, after separatory, oil reservoir dewaters, then through single pressing removing stearic acid, is separated and obtains thick oleic acid, and thick oleic acid is through distillation, cooling step, then through twice pressing, removing Palmiticacid, finally obtains oleic acid finished product.
Further, animal-plant oil for founding tallow 25-39%, found lard 11-15%, bone fat 35-39% and Oleum Gossypii semen 21-25%.
Further, refining purifying technique comprises filtration, comes unstuck and decolour; First stock oil is filtered, add water after filtration to stir and come unstuck for 1-2 hour, stirring velocity is less than 80 revs/min, the mass ratio [1-1.2] of stock oil and water: 1, water temperature is 20-30 DEG C, stratification after stirring, leaves standstill 5-8 hour, is separated, obtain lower floor's raw material oil reservoir, the moisture of raw material oil reservoir is less than 0.1%, if moisture is greater than 0.1% carry out decompression dehydration, until moisture is less than 0.1%; In stock oil, gac and carclazyte is added after coming unstuck, wherein the mass ratio of stock oil, gac and carclazyte is 1000:3:[10-20], bleaching temperature 80-110 DEG C, normal pressure decolours, stirring velocity is less than 80 rpms, bleaching time 10-30 minute, filter after decolouring purify after stock oil.
Further, dehydrating step be normal pressure dehydration, dehydration temperaturre 100-105 DEG C, dewater to the moisture in oleic acid be less than 0.2% stopping dehydration.
Further, the temperature of single pressing is 50-60 DEG C, and pressure is 1000-1050kg/cm
2, the time is 2-3 hour, and after single pressing, white soft small pieces are stearic acid, and oily liquids is thick oleic acid.
Further, thick oleic acid is through underpressure distillation, and vacuum tightness is at 200-300pa, and still is residual stops underpressure distillation when 3%-5%, and be cooled to 30-35 DEG C through twice pressing, obtain the scale Palmiticacid of white band pearly-lustre, oily liquids is finished product oleic acid.
Beneficial effect of the present invention:
The present invention produces the production technique of stearic acid and oleic acid, and technique is simple, and old lower, and oleic acid is separated comparatively thorough with stearic acid, constant product quality.Hydrolytic process technique of the present invention is simple, and easy to operate, hydrolysis time is short, and hydrolysis fully, can produce stearic acid and oleic acid simultaneously; The production technique that the present invention produces stearic acid and oleic acid is compared to the refining purification in the production technique of traditional stearic acid and oleic acid, hydrolysis, single pressing, dehydration, distillation, cooling, twice pressing and dehydrating step, lack last dehydrating step, and just dewatered before single pressing, and dehydration is comparatively thorough, moisture content in the stearic acid obtained is little, and product quality is high.
Embodiment
Embodiment 1
Found tallow 290g, found lard 120g, bone fat 360g, Oleum Gossypii semen 230g and emulsion 30g fully mix, first filtered by above-mentioned mixed solution, the object of filtration is removing mechanical impurity.Add 25 DEG C of water 1000g 70 revs/min stirring after filtration to come unstuck for 2 hours, leave standstill 8 hours after stirring, separatory obtains lower floor's raw material oil reservoir; The moisture of lower floor's raw material oil reservoir is 0.9%, and vacuum tightness is that 200pa carries out decompression dehydration, and decompression dehydration is after 15 minutes, and surveying stock oil moisture is 0.08%.In stock oil, add 3.09g gac and 16.5 carclazytes after coming unstuck, be warming up to 80 DEG C, normal pressure decolour, stirring velocity 60 rpms, bleaching time 15 minutes, filter after decolouring purify after stock oil.
Stock oil after purification adds 98% sulfuric acid 110g, water 825g, the temperature of reaction of controlled hydrolysis is 105 DEG C, the pressure of hydrolysis is at 68bar, the time of hydrolysis is 2.5 hours, stratification 5 hours after hydrolysis, and oil reservoir carries out normal pressure dehydration, dehydration temperaturre 100 DEG C, stops dehydration when to dewater to the moisture in oleic acid be 0.15%.
Carry out single pressing after dehydration, the temperature of single pressing is 50 DEG C, and pressure is 1050kg/cm
2, the squeezing time is 3 hours, and obtaining white soft small pieces after single pressing is stearic acid, and oily liquids is thick oleic acid.Described thick oleic acid is through underpressure distillation, and vacuum tightness is at 300pa, and still is residual stops underpressure distillation 3% time, and be cooled to 35 DEG C through twice pressing, obtain the scale Palmiticacid of white band pearly-lustre, oily liquids is finished product oleic acid.
Table 1 embodiment 1 stearic acid detected result
Table 2 embodiment 1 oleic acid detected result
Embodiment 2
Found tallow 250g, found lard 150g, bone fat 350g, Oleum Gossypii semen 250g and emulsion 50g fully mix, first filtered by above-mentioned mixed solution, the object of filtration is removing mechanical impurity.Add 25 DEG C of water 1100g 50 revs/min stirring after filtration to come unstuck for 1 hour, leave standstill 6 hours after stirring, separatory obtains lower floor's raw material oil reservoir; The moisture of lower floor's raw material oil reservoir is 1.0%, and vacuum tightness is that 300pa carries out decompression dehydration, and decompression dehydration is after 20 minutes, and surveying stock oil moisture is 0.07%.In stock oil, add 3.3g gac and 19.5 carclazytes after coming unstuck, be warming up to 100 DEG C, normal pressure decolour, stirring velocity 50 rpms, bleaching time 30 minutes, filter after decolouring purify after stock oil.
Stock oil after purification adds 95% sulfuric acid 105g, water 750g, the temperature of reaction of controlled hydrolysis is 115 DEG C, the pressure of hydrolysis is at 63bar, the time of hydrolysis is 2 hours, stratification 8 hours after hydrolysis, and oil reservoir carries out normal pressure dehydration, dehydration temperaturre 103 DEG C, stops dehydration when to dewater to the moisture in oleic acid be 0.15%.
Carry out single pressing after dehydration, the temperature of single pressing is 60 DEG C, and pressure is 1000kg/cm
2, the squeezing time is 2 hours, and obtaining white soft small pieces after single pressing is stearic acid, and oily liquids is thick oleic acid.Described thick oleic acid is through underpressure distillation, and vacuum tightness is at 200pa, and vinasse stops underpressure distillation 5% time, is cooled to 30 DEG C through twice pressing, and obtain the scale Palmiticacid of white band pearly-lustre, oily liquids is finished product oleic acid.
Table 3 embodiment 2 stearic acid detected result
Table 4 embodiment 2 oleic acid detected result
Embodiment 3
Found tallow 290g, found lard 110g, bone fat 390g, Oleum Gossypii semen 210g and emulsion 40g fully mix, first filtered by above-mentioned mixed solution, the object of filtration is removing mechanical impurity.Add 25 DEG C of water 1100g 50 revs/min stirring after filtration to come unstuck for 2 hours, leave standstill 7 hours after stirring, separatory obtains lower floor's raw material oil reservoir; The moisture of lower floor's raw material oil reservoir is 1.1%, and vacuum tightness is that 280pa carries out decompression dehydration, and decompression dehydration is after 15 minutes, and surveying stock oil moisture is 0.10%.In stock oil, add 3.3g gac and 19.5 carclazytes after coming unstuck, be warming up to 100 DEG C, normal pressure decolour, stirring velocity 50 rpms, bleaching time 30 minutes, filter after decolouring purify after stock oil.
Stock oil after purification adds 98% sulfuric acid 105g, water 750g, the temperature of reaction of controlled hydrolysis is 110 DEG C, the pressure of hydrolysis is at 68bar, the time of hydrolysis is 2.5 hours, stratification 8 hours after hydrolysis, and oil reservoir carries out normal pressure dehydration, dehydration temperaturre 105 DEG C, stops dehydration when to dewater to the moisture in oleic acid be 0.10%.
Carry out single pressing after dehydration, the temperature of single pressing is 60 DEG C, and pressure is 1050kg/cm
2, the squeezing time is 2 hours, and obtaining white soft small pieces after single pressing is stearic acid, and oily liquids is thick oleic acid.Described thick oleic acid is through underpressure distillation, and vacuum tightness is at 260pa, and vinasse stops underpressure distillation 4% time, is cooled to 35 DEG C through twice pressing, and obtain the scale Palmiticacid of white band pearly-lustre, oily liquids is finished product oleic acid.
Table 5 embodiment 3 stearic acid detected result
Table 6 embodiment 3 oleic acid detected result
Comparative example 1
Found tallow 290g, found lard 120g, bone fat 360g, Oleum Gossypii semen 230g and emulsion 30g fully mix, first filtered by above-mentioned mixed solution, the object of filtration is removing mechanical impurity.Add 25 DEG C of water 1000g 70 revs/min stirring after filtration to come unstuck for 2 hours, leave standstill 8 hours after stirring, separatory obtains lower floor's raw material oil reservoir; The moisture of lower floor's raw material oil reservoir is 0.9%, and vacuum tightness is that 200pa carries out decompression dehydration, and decompression dehydration is after 15 minutes, and surveying stock oil moisture is 0.08%.In stock oil, add 3.09g gac and 16.5 carclazytes after coming unstuck, be warming up to 80 DEG C, normal pressure decolour, stirring velocity 60 rpms, bleaching time 15 minutes, filter after decolouring purify after stock oil.
Stock oil after purification adds 98% sulfuric acid 110g, water 825g, and the temperature of reaction of controlled hydrolysis is 105 DEG C, and the pressure of hydrolysis is at 68bar, and the time of hydrolysis is 2.5 hours, stratification 5 hours after hydrolysis, separatory.
The oil reservoir that separatory obtains carries out single pressing, and the temperature of single pressing is 50 DEG C, and pressure is 1050kg/cm
2, the squeezing time is 3 hours, and obtaining white soft small pieces after single pressing is stearic acid, and oily liquids is thick oleic acid.Thick oleic acid carries out normal pressure dehydration, dehydration temperaturre 100 DEG C, stops dehydration when to dewater to the moisture in oleic acid be 0.15%.Through underpressure distillation after thick oleic acid dehydration, vacuum tightness is at 280pa, vinasse stops underpressure distillation 3% time, be cooled to 35 DEG C through twice pressing, obtain the scale Palmiticacid of white band pearly-lustre, oily liquids normal pressure dewaters, dehydration temperaturre 100 DEG C, stops dehydration being finished product oleic acid when to dewater to the moisture in oleic acid be 0.15%.
Table 7 comparative example 1 stearic acid detected result
Table 8 comparative example 1 oleic acid detected result
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (6)
1. a production technique for stearic acid and oleic acid, is characterized in that comprising the following steps: refining purification, hydrolysis, dehydration, single pressing, distillation, cooling and twice pressing; Described hydrolysing step is: select animal-plant oil and emulsion to be stock oil, the mass ratio 100:3-5 of animal-plant oil and emulsion, stock oil, the 95-98% vitriol oil and quality are than being 100:[10-11]: [71-78], the temperature of reaction of controlled hydrolysis is 105-115 DEG C, the pressure of hydrolysis is at 63-68bar, and the time of hydrolysis is 2-2.5 hour; After hydrolysis, standing separatory, after separatory, oil reservoir dewaters, then through single pressing removing stearic acid, is separated and obtains thick oleic acid, and thick oleic acid is through distillation, cooling step, then through twice pressing, removing Palmiticacid, finally obtains oleic acid finished product.
2. the production technique of a kind of stearic acid according to claim 1 and oleic acid, is characterized in that: described animal-plant oil for founding tallow 25-39%, found lard 11-15%, bone fat 35-39% and Oleum Gossypii semen 21-25%.
3. the production technique of a kind of stearic acid according to claim 1 and oleic acid, is characterized in that: described refining purifying technique comprises filtration, comes unstuck and decolour; First stock oil is filtered, add water after filtration to stir and come unstuck for 1-2 hour, stirring velocity is less than 80 revs/min, the mass ratio [1-1.2] of stock oil and water: 1, water temperature is 20-30 DEG C, stratification after stirring, leaves standstill 5-8 hour, is separated, obtain lower floor's raw material oil reservoir, the moisture of raw material oil reservoir is less than 0.1%, if moisture is greater than 0.1% carry out decompression dehydration, until moisture is less than 0.1%; In stock oil, gac and carclazyte is added after coming unstuck, wherein the mass ratio of stock oil, gac and carclazyte is 1000:3:[10-20], bleaching temperature 80-110 DEG C, normal pressure decolours, stirring velocity is less than 80 rpms, bleaching time 10-30 minute, filter after decolouring purify after stock oil.
4. the production technique of a kind of stearic acid according to claim 1 and oleic acid, is characterized in that: described dehydrating step be normal pressure dehydration, dehydration temperaturre 100-105 DEG C, dewater to the moisture in oleic acid be less than 0.2% stopping dehydration.
5. the production technique of a kind of stearic acid according to claim 1 and oleic acid, is characterized in that: the temperature of described single pressing is 50-60 DEG C, and pressure is 1000-1050kg/cm
2, the time is 2-3 hour, and after single pressing, white soft small pieces are stearic acid, and oily liquids is thick oleic acid.
6. the production technique of a kind of stearic acid according to claim 5 and oleic acid, it is characterized in that: described thick oleic acid is through underpressure distillation, vacuum tightness is at 200-300pa, still is residual stops underpressure distillation when 3%-5%, be cooled to 30-35 DEG C through twice pressing, obtain the scale Palmiticacid of white band pearly-lustre, oily liquids is finished product oleic acid.
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| CN201510261271.7A CN104946404A (en) | 2015-05-21 | 2015-05-21 | Production technology of stearic acid and oleic acid |
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| CN201510261271.7A CN104946404A (en) | 2015-05-21 | 2015-05-21 | Production technology of stearic acid and oleic acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106867601A (en) * | 2017-03-13 | 2017-06-20 | 宜兴市星光宝亿化工有限公司 | A kind of diesel antiwear additive and preparation method thereof |
| CN114426474A (en) * | 2021-11-25 | 2022-05-03 | 新疆华雄再生资源科技有限公司 | Preparation method of cottonseed oil and saponin biological stearic acid |
-
2015
- 2015-05-21 CN CN201510261271.7A patent/CN104946404A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106867601A (en) * | 2017-03-13 | 2017-06-20 | 宜兴市星光宝亿化工有限公司 | A kind of diesel antiwear additive and preparation method thereof |
| CN114426474A (en) * | 2021-11-25 | 2022-05-03 | 新疆华雄再生资源科技有限公司 | Preparation method of cottonseed oil and saponin biological stearic acid |
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Application publication date: 20150930 |