CN102329221A - Method for preparing isostearic acid - Google Patents
Method for preparing isostearic acid Download PDFInfo
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- CN102329221A CN102329221A CN201110194088A CN201110194088A CN102329221A CN 102329221 A CN102329221 A CN 102329221A CN 201110194088 A CN201110194088 A CN 201110194088A CN 201110194088 A CN201110194088 A CN 201110194088A CN 102329221 A CN102329221 A CN 102329221A
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Abstract
The invention relates to a method for preparing isostearic acid. The technical scheme is that the method comprises the following steps of: (1) producing dimer acid by using vegetable oil acid by a carclazyte catalysis method to obtain a byproduct, namely monomer acid; (2) controlling the temperature to be 90 to 98 DEG C and performing atmospheric esterification on the monomer acid and lower alcohol to obtain monomer acid ester by taking toluenesulfonic acid as a catalyst; (3) performing catalytic hydrogenation on the monomer acid ester to obtain aliphatic ester with a low iodine value; (4) sequentially saponifying and acidifying the aliphatic ester to obtain a mixture of stearic acid and isostearic acid; and (5) dissolving the mixture of the stearic acid and the isostearic acid by using No.6 solvent oil, reducing the temperature to -2 to 2 DEG C and performing cold separation, filtering, distilling filtrate under reduced pressure, and collecting fractions of the isostearic acid to obtain a finished product. Compared with the prior art, the method has the advantages that: the process is simple, equipment investment is low, and the safe operation is also ensured; an obtained product has high purity; and an acid value of the finished product is 180 to 188 mgKOH/g, and an iodine value is less than 8g/100g.
Description
Technical field
The present invention relates to a kind of Chemicals method of manufacture, particularly a kind of preparation method of Unimac 5680.
Background technology
At present, mostly be to synthesize the Unimac 5680 product, but the Unimac 5680 side chain that this synthesis method generates is longer, with natural acid very big-difference is arranged with Fatty Alcohol(C12-C14 and C12-C18), its purity does not reach the quality of natural Unimac 5680.
Also having other a kind of method of manufacture in addition in the industry, promptly is raw material with the vegetable oil acid, separation and Extraction Unimac 5680 in the by product monomer acids of employing carclazyte catalysis method synthesis of dimmer acid; And the production of step carclazyte catalysis method wherein dimeracid obtains the by product monomer acids by extensively open and use; Therefore the technology comparative maturity has document to disclose with the urea envelope method and directly extracts stearic method in the monomer acids, discloses a kind of with stearic method in the urea envelope method extraction monomer acids such as Chinese patent 200610097344.4; Its method is under the 30-80 temperature; With solvent urea is dissolved, add monomer acids backflow 0.5-5 hour, be chilled to after the room temperature to-10-20 ℃ cold analysis 1-20 hour; Obtain white adipose acid-urea inclusion and light yellow filtrating behind the suction filtration; Then filtrate decompression distillation is removed and desolvates, after the hot wash Unimac 5680, again in thermostat container with 30-100 ℃ of temperature under dry and obtain product.The shortcoming of this method is: the first, owing to there is unsaturated fatty acids such as calculation again in the monomer acids; And there is not the step of hydrogenation in the technology; The iodine number of the product that therefore obtains is high, and the antioxidant property of product is low, and the color of product deepens easily; The second, Unimac 5680 and Triple Pressed Stearic Acid iodine number difference are very little, and the isolating effect of urea envelope is undesirable.
Defective to aforesaid method; Chinese patent 200910042703.X discloses the separating and extracting method of Unimac 5680 in a kind of monomer acids; Its method is the by product monomer acids when oleic acid, linolic acid carclazyte catalysis method are produced dimeracid, at first passes through the esterification of catalyst-free middle-pressure process, presses shortening in then the monomer acid esters being adopted; In solvent, obtain the isostearate bullion again through the separation of urea envelope; Again bullion is obtained refining isostearate through short-path distillation, obtain Unimac 5680 through alkali and acid hydrolysis again, obtain the Unimac 5680 product after dehydrating.Because study on mechanism such as the hydrogenation of the esterification of higher fatty acid and high-grade aliphatic ester, hydrolysis are more deep, technology is comparative maturity also, through hydrogenation reaction; Make saturated lipid acid such as unsaturated acid hydrogenation generation Triple Pressed Stearic Acid such as oleic acid, reduced the iodine number of product, improved the oxidation-resistance of product; But still there is following shortcoming: the first, by product monomer acids; If use the middle-pressure process esterification, working pressure is high, needs to use explosion-proof pressure reactor; Fund input is bigger, also is unfavorable for safety operation simultaneously; The second, the iodine number difference of the stearate of hydrogenation generation and isostearate is very little, and the isolating effect of urea envelope is undesirable.
Summary of the invention
The object of the invention is exactly the defective that exists to prior art; Step and controlled variable to prior art are improved; Process step is by middle pressure esterification-hydrogenation-urea envelope-refining-hydrolysis; Be improved to normal pressure esterification-hydrogenation-saponification-acidifying-crystallization and purification-distillation and purify, simultaneously processing parameter is adjusted, provide that a kind of technology is simple, product purity is high, the Unimac 5680 method for manufacturing of operational safety.
The present invention realizes through following technical scheme: may further comprise the steps
(1) vegetable oil acid carclazyte catalysis method is produced dimeracid and obtain the by product monomer acids;
(2) make catalyzer with tosic acid, 90～98 ℃ of temperature controls, monomer acids and lower alcohol carry out normal pressure esterification and generate the monomer acid esters;
(3) monomer acid esters shortening obtains the fatty ester of low iodine number;
(4) fatty ester obtains low iodine number fatty acid mixt successively through saponification, acidification;
(5) after low iodine number fatty acid mixt dissolved with No. six solvent oils, Jiang Wen with the filtrate decompression distillation, collected the cut of Unimac 5680, thereby obtains finished product after the filtration Dao 2 ℃～2 ℃ cold analysis of –.
In order to reach better reaction effect, the preferred version of such scheme is following:
(1) vegetable oil acid adopts acidic white earth as catalyzer, is being lower than polyreaction under 245 ℃ of conditions, and carclazyte is removed in press filtration, and the filtrate decompression distillation obtains the cut of monomer acids;
(2) make catalyzer with tosic acid, temperature control 90-98 ℃, monomer acids and lower alcohol carry out normal pressure esterification and generate the monomer acid esters, and reaction time of esterification is lower than 5 g/100g with the acid number of resultant and is as the criterion, and esterification finish after washing, and the static layering disacidify is mixed;
(3) the monomer acid esters is under N120 type catalyst action, and pressure-controlling is between 1.5MPa～2.2 MPa, and 190～220 ℃ of temperature controls fed hydrogen reaction 4～8 hours, were cooled to 90 ℃ Celsius again, filtered out catalyzer, promptly got the fatty ester that hangs down iodine number;
(4) by low iodine number fatty ester weight 20～30% to wherein adding concentration 10～15% sodium hydroxide solutions, heat up and boiled 3～4 hours, and 95 ℃ of insulations 6～8 hours; Be cooled to 40 ℃ Celsius, emit alcohol-water mixture, after lower alcohol was reclaimed in distillation, adding concentration was 25～40% sulphuric acid solns, and consumption is transferred to 2～3 with pH value and is got final product, boiled again 1～3 hour, and 95 ℃ of insulations 5～8 hours; Be cooled to 45～55 ℃ again, left standstill 6 hours, put sour water, and leftover materials are washed to pH value equal 7, obtain low iodine number fatty acid mixt;
(5) low iodine number fatty acid mixt and No. six solvent oils are by weight 2 ℃～2 ℃ of the mixed Leng Dong Zhi – of 1:3, filtration; Filtrating is sent into stainless steel tubulation vacuum climbing-film evaporation operation, under vacuum tightness 1500Pa and 100～130 ℃ of conditions, sloughs solvent, and reclaims solvent; Send into high vacuum tubulation falling-film distillation operation again, the Unimac 5680 cut is collected in distillation under the condition of condition of high vacuum degree 15-25Pa and 220-280 ℃; Solvent-laden filter cake is sent into stainless steel falling liquid film vacuum-evaporation operation, is cooled to 70 ℃ after under 130 ℃ and vacuum condition, sloughing solvent, sends into the slicing machine section, promptly gets Triple Pressed Stearic Acid.
In order better to realize the present invention; The further preferred version of such scheme also comprises: described step (1) vegetable oil acid is made catalyzer with carclazyte under 220～224 ℃ of conditions, synthesis under normal pressure adds phosphoric acid after 4 hours and removes metal complex; Carclazyte is removed in press filtration; Filtrate decompression distillation in vacuum tightness 8-12Pa and liquid phase 220-260 ℃, is collected the cut of monomer acids.
The cotton seed oleic acid of the preferred zero pour of vegetable oil acid in the said step (1)≤8 ℃, catalyzer also comprises Quilonum Retard, improves speed of response; Lower alcohol in the step (2) is a methyl alcohol, and reaction time of esterification is 3-10 hour, and this reaction times is corresponding with the acid number detection, and esterification time is in 3-10 hour under normergic situation, and acid number all can be lower than 5 g/100g.
The present invention compared with prior art, technology is simple, through selecting suitable catalyzer for use; Adopt the non-pressure process esterification, facility investment is few, also helps safety operation simultaneously; After improving process step simultaneously, the difference of Triple Pressed Stearic Acid and Unimac 5680 solubleness in No. six solvent oils be can utilize, Triple Pressed Stearic Acid and Unimac 5680 separated through the cooling cold analysis; And through the rectification and purification Unimac 5680, the product yield that this kind method obtains is high, purity is high, and its acid number is 180～188mgKOH/g; Iodine number is less than 8 mgKOH/g, and zero pour is less than 8 ℃; Simultaneously can also obtain up-to-standard by product Triple Pressed Stearic Acid, its acid number 190～203 mgKOH/g, iodine number are less than 4 mgKOH/g, zero pour >=55 ℃, remarkable in economical benefits.
Embodiment
Embodiment 1
The preparation method of Unimac 5680 may further comprise the steps:
(1) vegetable oil acid adopts acidic white earth as catalyzer, polyreaction under 220 ℃ of conditions, and synthesis under normal pressure adds phosphoric acid after 4 hours and removes metal complex;, carclazyte is removed in press filtration, the filtrate decompression distillation; In 240 ℃ of vacuum tightness 10Pa and liquidus temperatures, collect the cut of monomer acids;
(2) make catalyzer with tosic acid, 90 ℃ of temperature controls, monomer acids and methyl alcohol carry out normal pressure esterification, react 10 hours, and iodine number is 4.8 g/100g, promptly generates the monomer acid esters; Esterification finishes after washing, and the static layering disacidify is assorted;
(3) the monomer acid esters is under N120 type catalyst action, and pressure-controlling is at 1.5 ~ 2.2MPa MPa, and 190 ℃ of temperature controls fed hydrogen reaction after 8 hours, were cooled to 90 ℃ again, filtered out catalyzer, promptly got the fatty acid methyl ester that hangs down iodine number;
(4) dissolve to wherein adding concentration 15% hydroxide by 20% of the weight of low iodine number fatty acid methyl ester, heat up and boiled 4 hours, 95 ℃ of insulations 6 hours; Be cooled to 40 ℃, emit alcohol-water mixture, after methyl alcohol was reclaimed in distillation, adding concentration was 25～40% sulphuric acid solns, transferred pH value to 2 to get final product, and boiled 1 hour again, and 95 ℃ are incubated 8 hours; Be cooled to 45～55 ℃ again, left standstill 6 hours, put sour water, and material washed to pH value equal 7, obtain low iodine number fatty acid mixt;
(5) low iodine number fatty acid mixt and No. six solvent oils after the mixed dissolving of 1:3, are refrigerated to 2 ℃～2 ℃ of She Shi –, vacuum filtration.
Filtrating is sent into stainless steel tubulation vacuum climbing-film evaporation operation, under 100～130 ℃ and vacuum 1500Pa condition, sloughs and reclaim solvent oil; Send into high vacuum tubulation falling-film distillation operation again, be collected in the Unimac 5680 cut under high vacuum 20Pa and the 250 ℃ of conditions, thereby obtain the finished product of acid number 188KOH/g, iodine number 7.50 g/100g.
Solvent-laden filter cake is sent into stainless steel falling liquid film vacuum-evaporation operation, is cooled to 70 ℃ after under 130 ℃ and vacuum condition, sloughing solvent, sends into the slicing machine section, promptly gets Triple Pressed Stearic Acid, its index; Acid number 190mgKOH/g, iodine number 3.8 g/100g, 60 ℃ at zero pour.
Embodiment 2
The preparation method of Unimac 5680 may further comprise the steps:
(1) vegetable oil acid adopts acidic white earth as catalyzer, polyreaction under 224 ℃ of conditions, and the polymerization under atmospheric pressure reaction adds phosphoric acid after 4 hours and removes metal complex;, carclazyte is removed in press filtration, the filtrate decompression distillation; When being collected in 240 ℃ of vacuum 10Pa and liquidus temperatures, collect the cut of monomer acids;
(2) make catalyzer with tosic acid, 98 ℃ of temperature controls, monomer acids and methyl alcohol carry out normal pressure esterification, react 3 hours, and iodine number is 4.5 g/100g, promptly generates the monomer acid esters; Esterification finishes after washing, and the deposition disacidify is assorted;
(3) the monomer acid esters is under effect under the N120 type catalyst action, and pressure-controlling is at 1.5 ~ 2.2MPa MPa, and 220 ℃ of temperature controls fed hydrogen reaction 4 hours, were cooled to 90 ℃ again, filtered out catalyzer, promptly got the fatty acid methyl ester that hangs down iodine number;
(4) dissolve to wherein adding concentration 10% hydroxide by 30% of low iodine number fatty acid methyl ester weight, heat up and boiled 3 hours, and 95 ℃ of insulations 8 hours; Be cooled to 40 ℃, emit alcohol-water mixture, after methyl alcohol was reclaimed in distillation, adding concentration was 25～40% sulphuric acid solns, transferred pH value to 3 to get final product, and boiled 3 hours again, and 95 ℃ are incubated 5 hours; Be cooled to 45～55 ℃ again, left standstill 6 hours, put sour water, and material washed to pH value equal 7, obtain low iodine number fatty acid mixt;
(5) low iodine number fatty acid mixt and No. six solvent oils after the mixed dissolving of 1:3, are refrigerated to 2 ℃～2 ℃ of She Shi –, vacuum filtration.
Filtrating is sent into stainless steel tubulation vacuum climbing-film evaporation operation, under 100～130 ℃ and vacuum 1500Pa condition, sloughs and reclaim solvent oil; Send into high vacuum tubulation falling-film distillation operation again, be collected in the Unimac 5680 cut under high vacuum 20Pa and the 250 ℃ of conditions, thereby obtain acid number 180mgKOH/g, iodine number 7.56 g/100g finished products.
Solvent-laden filter cake is sent into stainless steel falling liquid film vacuum-evaporation operation, is cooled to 70 ℃ after under 130 ℃ and vacuum condition, sloughing solvent, sends into the slicing machine section, promptly gets Triple Pressed Stearic Acid, its index; Acid number 203mgKOH/g, iodine number 3.5g/100g, 55 ℃ at zero pour.
Embodiment 3
The preparation method of Unimac 5680 may further comprise the steps:
(1) vegetable oil acid adopts acidic white earth as catalyzer, polyreaction under preparing method's ℃ condition of Unimac 5680, and synthesis under normal pressure adds phosphoric acid after 4 hours and removes metal complex; Carclazyte is removed in press filtration, and filtrating is collected the cut of monomer acids in 240 ℃ of vacuum 10Pa and liquidus temperatures;
(2) make catalyzer with tosic acid, 90 ℃ of temperature controls, monomer acids and methyl alcohol carry out normal pressure esterification, react 10 hours, and iodine number is 4.3 g/100g, promptly generates the monomer acid esters; Esterification finishes after washing, and the static layering disacidify is assorted;
(3) the monomer acid esters is under effect under the N120 type catalyst action, and pressure-controlling is at 1.5 ~ 2.2MPa MPa, and 190 ℃ of temperature controls fed hydrogen reaction after 6 hours, were cooled to 90 ℃ again, filtered out catalyzer, promptly got the fatty acid methyl ester that hangs down iodine number;
(4) dissolve to wherein adding concentration 15% hydroxide by 25% of low iodine number fatty acid methyl ester weight, heat up and boiled 3.5 hours, and 95 ℃ of insulations 7 hours; Be cooled to 40 ℃, emit alcohol-water mixture, after methyl alcohol was reclaimed in distillation, adding concentration was 25～40% sulphuric acid solns, transferred pH value to 2.5 to get final product, and boiled 2 hours again, and 95 ℃ are incubated 6.5 hours; Be cooled to 45～55 ℃ again, left standstill 6 hours, put sour water, and material washed to pH value equal 7, obtain low iodine number fatty acid mixt;
(5) low iodine number fatty acid mixt and No. six solvent oils after the mixed dissolving of 1:3, are refrigerated to 2 ℃～2 ℃ of She Shi –, vacuum filtration;
Filtrating is sent into stainless steel tubulation vacuum climbing-film evaporation operation, under 100～130 ℃ and vacuum 1500Pa condition, sloughs and reclaim solvent oil; Send into high vacuum tubulation falling-film distillation operation again, be collected in the Unimac 5680 cut under high vacuum 20Pa and the 250 ℃ of conditions, thereby obtain the Unimac 5680 finished product of acid number 184 mgKOH/g, iodine number 7.52 g/100g.
Solvent-laden filter cake is sent into stainless steel falling liquid film vacuum-evaporation operation, is cooled to 70 ℃ after under 130 ℃ and vacuum condition, sloughing solvent, sends into the slicing machine section, promptly gets Triple Pressed Stearic Acid, its index; Acid number 196 mgKOH/g, iodine number 3.7 g/100g, 65 ℃ at zero pour.
Embodiment 4
The preparation method of Unimac 5680; In embodiment 1 step (1), increase the Quilonum Retard catalyzer, improve speed of response, other steps remain unchanged; Finally obtain the Unimac 5680 finished product of acid number 187KOH/g, iodine number 7.44 g/100g; Its index of by product Triple Pressed Stearic Acid: acid number 195 mgKOH/g, iodine number 3.6g/100g, 62 ℃ at zero pour.
Embodiment 5
The preparation method of Unimac 5680; In embodiment 2 steps (1), increase the Quilonum Retard catalyzer, improve speed of response, other steps remain unchanged; Finally obtain the Unimac 5680 finished product of acid number 186mgKOH/g, iodine number 7.46 g/100g; Its index of by product Triple Pressed Stearic Acid: acid number 196 mgKOH/g, iodine number 3.9g/100g, 61 ℃ at zero pour.
Embodiment 6
The preparation method of Unimac 5680; In embodiment 3 steps (1), increase the Quilonum Retard catalyzer, improve speed of response, other steps remain unchanged; Finally obtain the Unimac 5680 finished product of acid number 186KOH/g, iodine number 7.45 g/100g; Its index of by product Triple Pressed Stearic Acid: acid number 193 mgKOH/g, iodine number 3.7g/100g, 58 ℃ at zero pour.
Embodiment 7
The preparation method of Unimac 5680; Vegetable oil acid in embodiment 1 step (1) is preferably zero pour less than 8 ℃ cotton seed oleic acid; Other steps are constant, finally obtain the Unimac 5680 finished product of acid number 188KOH/g, iodine number 7.20g/100g, its index of by product Triple Pressed Stearic Acid: acid number 194mgKOH/g; Iodine number 3.59g/100g, 59 ℃ at zero pour.
Embodiment 8
The preparation method of Unimac 5680; Vegetable oil acid in embodiment 2 steps (1) is preferably zero pour less than 8 ℃ cotton seed oleic acid; Other steps are constant, finally obtain the Unimac 5680 finished product of acid number 187KOH/g, iodine number 7.10g/100g, its index of by product Triple Pressed Stearic Acid: acid number 201 mgKOH/g; Iodine number 3.5g/100g, 64 ℃ at zero pour.
Embodiment 9
The preparation method of Unimac 5680; Vegetable oil acid in embodiment 3 steps (1) is preferably zero pour less than 8 ℃ cotton seed oleic acid; Other steps are constant, finally obtain the Unimac 5680 finished product of acid number 186KOH/g, iodine number 7.21g/100g, its index of by product Triple Pressed Stearic Acid: acid number 202 mgKOH/g; Iodine number 3.5g/100g, 65 ℃ at zero pour.
Embodiment 10
The preparation method of Unimac 5680; Methyl alcohol in embodiment 1 step (2) is changed to butanols; Other steps are constant, finally obtain the Unimac 5680 finished product of acid number 182KOH/g, iodine number 7.74 g/100g, its index of by product Triple Pressed Stearic Acid: acid number 196 mgKOH/g; Iodine number 3.9g/100g, 56 ℃ at zero pour.
Embodiment 11
The preparation method of Unimac 5680; Methyl alcohol in embodiment 2 steps (2) is changed to Virahol; Other steps are constant, finally obtain the Unimac 5680 finished product of acid number 183KOH/g, iodine number 7.60 g/100g, its index of by product Triple Pressed Stearic Acid: acid number 195 mgKOH/g; Iodine number 3.7g/100g, 58 ℃ at zero pour.
Embodiment 12
The preparation method of Unimac 5680; Methyl alcohol in embodiment 2 steps (2) is changed to ethanol; Other steps are constant, finally obtain the Unimac 5680 finished product of acid number 184KOH/g, iodine number 7.56 g/100g, its index of by product Triple Pressed Stearic Acid: acid number 196 mgKOH/g; Iodine number 3.6g/100g, 57 ℃ at zero pour.
Above embodiment only is the preferred embodiments of the present invention, can realize best-of-breed technology effect of the present invention.Within protection scope of the present invention; Those skilled in the art can adopt other technical parameter to realize fully, such as hydrogenation according to the catalyzer of selecting other, such as rhodium, platinum etc.; And select corresponding temperature of reaction, pressure; The appropriateness adjustment of the processing parameter of the saponification of monomer acid esters and acidifying for another example, carclazyte catalytic production dimeracid etc., all identical with technical scheme substance of the present invention, therefore in this embodiment, do not enumerate one by one.
Claims (6)
1. the preparation method of Unimac 5680 is characterized in that, may further comprise the steps:
(1) vegetable oil acid carclazyte catalysis method is produced dimeracid and obtain the by product monomer acids;
(2) make catalyzer with tosic acid, temperature control 90-98 ℃, monomer acids and lower alcohol carry out normal pressure esterification and generate the monomer acid esters;
(3) monomer acid esters shortening obtains the fatty ester of low iodine number;
(4) fatty ester of low iodine number obtains low iodine number lipid acid miscellany successively through saponification, acidification;
(5) after low iodine number fatty acid mixt dissolved with No. six solvent oils, 2 ℃～2 ℃ crystallizations of Jiang Wen – with the filtrate decompression distillation, were collected the cut of Unimac 5680, thereby are obtained finished product after the filtration.
2. the preparation method of Unimac 5680 according to claim 1 is characterized in that, described step preferred version is:
(1) vegetable oil acid adopts acidic white earth as catalyzer, is being lower than polyreaction under 245 ℃ of conditions, and carclazyte is removed in press filtration, and the filtrate decompression distillation obtains the cut of monomer acids;
(2) make catalyzer with tosic acid, temperature control 90-98 ℃, monomer acids and lower alcohol carry out normal pressure esterification and generate the monomer acid esters, and reaction time of esterification is lower than 5 g/100g with the acid number of resultant and is as the criterion, and esterification finish after washing, and the static layering disacidify is mixed;
(3) the monomer acid esters is under N120 type catalyst action, and pressure-controlling is between 1.5MPa～2.2 MPa, and 190～220 ℃ of temperature controls fed hydrogen reaction 4～8 hours, were cooled to 90 ℃ Celsius again, filtered out catalyzer, promptly got the fatty ester that hangs down iodine number;
(4) by low iodine number fatty ester weight 20～30% to wherein adding concentration 10～15% sodium hydroxide solutions, heat up and boiled 3～4 hours, and 95 ℃ of insulations 6～8 hours; Be cooled to 40 ℃ Celsius, emit alcohol-water mixture, after lower alcohol was reclaimed in distillation, adding concentration was 25～40% sulphuric acid solns, and consumption is transferred to 2～3 with pH value and is got final product, boiled again 1～3 hour, and 95 ℃ of insulations 5～8 hours; Be cooled to 45～55 ℃ again, left standstill 6 hours, put sour water, and leftover materials are washed to pH value equal 7, obtain low iodine number fatty acid mixt;
(5) low iodine number fatty acid mixt and No. six solvent oils are by weight 2 ℃～2 ℃ of the mixed Leng Dong Zhi – of 1:3; Filter; Filtrating is sent into stainless steel tubulation vacuum climbing-film evaporation operation, under vacuum tightness 1500Pa and 100～130 ℃ of conditions, sloughs and reclaim solvent oil; Send into high vacuum tubulation falling-film distillation operation again, the Unimac 5680 cut is collected in distillation under the condition of condition of high vacuum degree 15-25Pa and 220-280 ℃.
3. the preparation method of the Unimac 5680 of stating according to claim 2; It is characterized in that: the preferred version of described step (1) is that vegetable oil acid is under 220～224 ℃ of conditions; Synthesis under normal pressure adds phosphoric acid after 4 hours and removes metal complex, and carclazyte is removed in press filtration, the filtrate decompression distillation; In vacuum tightness 8-12Pa and liquidus temperature 220-260 ℃, collect the cut of monomer acids.
4. the preparation method of Unimac 5680 according to claim 2 is characterized in that: reaction time of esterification is 3-10 hour in the described step (2).
5. according to the preparation method of the described Unimac 5680 of the arbitrary claim of 1-4, it is characterized in that: the catalyzer in the said step (1) also comprises Quilonum Retard, and the lower alcohol in the step (2) is a methyl alcohol.
6. according to the preparation method of the described Unimac 5680 of the arbitrary claim of 1-4, it is characterized in that: the vegetable oil acid in the said step (1) is the cotton seed oleic acid of zero pour≤8 ℃.
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| CN114573451A (en) * | 2022-02-16 | 2022-06-03 | 华南理工大学 | Method for separating 12-hydroxystearic acid, gamma-oleic acid lactone and delta-oleic acid lactone |
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| CN108342926A (en) * | 2017-12-30 | 2018-07-31 | 苏州丰倍生物科技有限公司 | A kind of environment-friendly type impact paper solvent and preparation method thereof |
| CN108299188A (en) * | 2018-03-12 | 2018-07-20 | 徐州市腾顺工贸有限公司 | A kind of freezing and crystallizing point puies forward the stearic preparation method of isomery |
| CN110252098A (en) * | 2018-03-12 | 2019-09-20 | 山东奥古生物科技有限公司 | A kind of air cleaning cream and preparation method thereof |
| CN114573451A (en) * | 2022-02-16 | 2022-06-03 | 华南理工大学 | Method for separating 12-hydroxystearic acid, gamma-oleic acid lactone and delta-oleic acid lactone |
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