CN102964245B - Preparation method of high-quality glycerin monostearate - Google Patents
Preparation method of high-quality glycerin monostearate Download PDFInfo
- Publication number
- CN102964245B CN102964245B CN201210501481.5A CN201210501481A CN102964245B CN 102964245 B CN102964245 B CN 102964245B CN 201210501481 A CN201210501481 A CN 201210501481A CN 102964245 B CN102964245 B CN 102964245B
- Authority
- CN
- China
- Prior art keywords
- distillation
- glyceryl monostearate
- feed liquid
- quality
- obtains
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The invention discloses a preparation method of high-quality glycerin monostearate. The method comprises the steps of reacting hydrogenated palm oil and glycerol under strong base catalysis to generate ester, and carrying out four-stage distillation to obtain high-quality glycerin monostearate. The acid value of the product is reduced to below 0.4, the freezing point is raised to 64-66 DEG C, the quality of the product is improved, and the difficulty of the prior art is overcome. Besides, the problems in the prior art that the pipeline is blocked by slag produced in the distillation process, the production efficiency is lowered, the product quality is reduced, the production is discontinuous and the processing efficiency is low resulting from scaling of an evaporating surface and a condensing surface are solved. Glycerol and hydrogenated palm oil can be recycled, so that the cost is low, the yield is high, the product quality is improved, and the whole processing controllability is high. The high-quality glycerin monostearate is suitable for industrial production.
Description
Technical field
The present invention relates to the invention belongs to the field of chemical synthesis, be specifically related to a kind of preparation method of high quality glyceryl monostearate.
Background technology
Glyceryl monostearate is a kind of white wax sheet, pearl or powdery solid, dissolves in the organic solvents such as chloroform, ethanol, acetone or ether, also dissolves in mineral oil and vegetable and animals oils.Water insoluble, strongly vibrating to mix with hot water dispersibles in hot water, also can form gel with hot water.Mono-glycerides HLB value, 3～4, belongs to water-in-oil (W/O) type emulsifying agent, because emulsifying property is unique, also can be used as oil-in-water (O/W) type emulsifying agent.China national standard < < foodstuff additive are used hygienic standard > > (GB2760-1996) regulation mono-glycerides to be used for varieties of food items by need of production, the foodstuff additive joint specialist council of Food and Argriculture OrganizationFAO and the World Health Organization (FAO/WHO) (JECFA) is decided to be " not limitting use " (no limit), and food and drug administration (FDA) assert and to be that " It is generally accepted into safety " (GRAS).
Glyceryl monostearate is a kind of tensio-active agent of non-ionic type.It existing hydrophilic have again oleophilic group because of, there is the several functions such as wetting, emulsification, foaming.
Glyceryl monostearate is emulsifying agent and the additive of food; In makeup and medical paste, be used as emulsifying agent, make lotion fine and smooth, lubricious; For the emulsifying agent of industrial yarn finish and the lubricant of textiles; In plastics film, be used as drip agent and antifogging agent; In plastic working, make lubricant and static inhibitor, can be used as in other respects defoamer, dispersion agent, thickening material, wetting agent etc.
Its preparation is generally and is divided into chemical method and biological process, and wherein chemical method has following several approach:
(1) by glycerine and stearic acid esterification and obtain.
Stearic acid, glycerine and sodium hydroxide are added in reactor, after heating and melting, start stirring, pass into nitrogen.Reacting by heating.This process application is the most general, but in technique, control condition is the key of product yield and purity, need to continue perfect.
(2) direct esterification
Stearic acid and glycerine are pressed 1:(1.2～1.3) mol ratio, under 0.2% an acidic catalyst effect, at 180～250 ℃: reaction 2～4h; Reactant speed is chilled to 100 ℃, adds alkali catalyst neutralisation, must be containing the product of monoesters 40%～60% after washing with water.This process yield is low, and product purity is low, aftertreatment difficulty, and relative cost is high.
(3) ester-interchange method
Stearin and glycerine are at 0.06%～0.1% Cu (OH)
2under existence, at 170～240 ℃ of reaction 1～2h, pass into nitrogen protection in reaction process, reactant obtains the product containing monoesters 40%～60% after decompression deodorization, acid neutralize, refine.This technique can be converted into glyceryl monostearate by many stearins, but scale is limited, and product yield is low, and cost is high.
(4) Racemic glycidol saponification method
Racemic glycidol and stearic acid, under the catalysis of tetraethyl ammonium iodide, at 100～130 ℃ of reaction 30～70min, can contain the product of monoesters 80%～90% after reactant is refining.This technological reaction mild condition, productive rate is high, but cost is higher.
(5) epoxy chloropropane phase transfer catalysis process
Epoxy chloropropane and sodium stearate (2:1, mol ratio) are in toluene, under the catalysis of phase-transfer catalyst Tetrabutyl amonium bromide, at 90～110 ℃ of reaction 2h; Reactant washs with sodium chloride solution, divides and gets organic phase, and toluene is removed in distillation and unreacted epoxy chloropropane obtains stearic acid glycidyl ester, used the NaOH solution hydrolysis of 0.1mol/L, through separated, dry, with normal hexane recrystallization, obtain product, monoester content is more than 90%.The monoesters product of content 40%～60% can obtain more than 90% high density product through molecular distillation.The productive rate of this technique is low, and cost is high.
Biological rule adopts the synthetic glyceryl monostearate of enzyme process to be, use lipase as a kind of efficient biological catalyst (Peng Lifeng. Food science [J], 1999,04), product not only has highly-solid selectively and regiospecificity, can synthetic chemistry method be difficult to synthetic optical purity product, but long reaction time, generally all more than 10 hours, and subsequent disposal expense is higher.
The quality of glyceryl monostearate product is directly connected to its safety applications in the fields such as medicine, food, makeup.In prior art, the standard that product can reach is iodine number (g I2/100g)≤2.0, acid number (mg KOH/g)≤2.0,60 ℃ of zero pour 55 –, saponification value (mg KOH/g) 160-175.Wherein acid number only can be controlled at below 2.0, conventionally more than 1.0.The requirement to the demand of glyceryl monostearate especially quality along with food and pharmaceutical prod, we further promote the quality of glyceryl monostearate an urgent demand.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of high yield, high quality, low cost, easy industrialized glyceryl monostearate preparation method are provided.
This object is achieved by following technical solution.This technical scheme is for esterification under base catalysis is synthetic, prepare high-quality glyceryl monostearate through the technique of level Four distilation.
This technique comprises the steps:
1) preparation of glyceryl monostearate crude product
First, glycerine is joined in esterification reaction tank, then catalyzer is slowly joined in esterification reaction tank, then be warming up to 90 degrees Celsius, stir 30 minutes;
Secondly, hydrogenated liquid plam oil is joined in above-mentioned esterification reaction tank, be fully uniformly mixed, be warmed up to T
0for 210-220 ℃, control pressure P is-0.06Mpa is to-0.09Mpa, carries out esterification 30min, obtains glyceryl monostearate crude product;
Wherein, described T
0be preferably 215-220 ℃, more preferably 218 ℃;
Described catalyzer is sodium hydroxide or potassium hydroxide, preferably sodium hydroxide.
Described catalyzer and the mass ratio of glycerine are (0.1-0.5): 100, be preferably (0.2-0.4): and 100,0.275:100 more preferably.
Described hydrogenated palm kernel oil is 1:(0.98-1.3 with the ratio of the amount of substance of glycerine); Be preferably 1:(1.0-1.1), 1:1.05 more preferably.
2) neutralizing treatment
In above-mentioned reacted glyceryl monostearate crude product, add phosphoric acid, adjusting pH is 6.0-7.5, is preferably 7.0, stir 15 minutes, and deslagging after standing 2 hours then, filtrate is the thick ester of glyceryl monostearate;
3) one-level distillation
By step 2) in the thick ester of glyceryl monostearate distill, distillation condition is as follows: temperature T
1for 160-225 ℃, preferred T
1be 170 ℃, vacuum P
1for 150-200pa, preferred P
1for 200pa, thermal oil pressure 0.25-0.3MPA.Steaming is removed most of moisture till extremely steaming without cut, obtains one-level distillation feed liquid.
This step is steamed except the moisture in feed liquid.
4) secondary distillation
By steaming one-level distillation feed liquid in step 3), carry out second stage distillation, distillation condition is: temperature T
2for 190-220 ℃, preferred T
2be 195 ℃, vacuum P
2for 3-10pa, preferred P
2for 10pa, thermal oil pressure 0.25-0.3MPA.Steaming is steamed except most glycerine and free fatty acids till extremely steaming without cut, obtains secondary distillation feed liquid.
5) three-stage distillation
Secondary distillation feed liquid in step 4) is carried out to three-stage distillation, and distillation condition is: temperature T
3for 200-220 ℃, preferred T
3be 210 ℃, vacuum P
3for 3-15pa, preferred P
3for 8pa, thermal oil pressure 0.25-0.3MPA.Steaming is extracted micro-glycerine and free fatty acids till extremely steaming without cut, obtains three-stage distillation feed liquid.
6) level Four distillation:
Three-stage distillation feed liquid in step 5) is carried out to level Four distillation, and distillation condition is: temperature T
4for 210-230 ℃, vacuum P
4for 0.1-7pa, thermal oil pressure 0.25-0.3MPA.Steaming obtains quality glyceryl monostearate liquid till extremely steaming without cut.
7) glyceryl monostearate liquid spray is cooling, pack to obtain glyceryl monostearate finished product.
The present invention utilizes reaction equation, reaction equilibrium constant and test practice, determines and produces prescription proportional quantity and the length in reaction times, controls preferably the main quality index such as acid number.In process of production, the parameters such as each material consumption, reaction times, technological temperature, vacuum tightness are controlled effectively, allow material complete reaction, fully purify.
Quality examination result of the present invention is:
Iodine number (gI
2/ 100g)≤2.0; Acid number (mg KOH/g)≤1.0; Zero pour: 64-65 ℃; Saponification value (mg KOH/g): 160-1750-175.Content >=99.9%.
The acid number of product of the present invention is down to below 0.3, and zero pour is increased to 64-66 ℃, has promoted the quality of product, has overcome the bottleneck difficult point of prior art.
Technical scheme provided by the invention is equally applicable to the preparation of the monoglyceride of high quality lauric acid, tetradecanoic acid, palmitinic acid, pearly-lustre resin acid, eicosanoic acid.
Compared with prior art, the present invention has following beneficial effect:
1) the present invention uses highly basic as catalyzer, and cost is lower, and easily separated.
2) the present invention adopts level Four distillation method, and whole glycerine and the free hydrogenated palm kernel oil going out be can be recycled, cost-saving.
3) quality product is high, yield is high, and whole process controllability is high, is applicable to industrial production.
Embodiment
Following content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; can also make some simple deduction or replace; all should be considered as belonging to protection scope of the present invention; the present invention uses but the technology and the indexing section that do not describe, is prior art.
embodiment 1
Prepare high-quality glyceryl monostearate, concrete technology is as follows:
1) preparation of glyceryl monostearate crude product
The preparation of step 1) glyceryl monostearate crude product:
First, 122kg glycerine is joined in esterification reaction tank, then 0.6kg sodium hydroxide slowly joins in esterification reaction tank, then is warming up to 90 degrees Celsius, stirs 30 minutes;
Secondly, 500kg hydrogenated liquid plam oil is joined in above-mentioned esterification reaction tank, be fully uniformly mixed, be warmed up to T
0be 210 ℃, control pressure P is-0.06Mpa, carries out esterification 30min, obtains glyceryl monostearate crude product;
2) neutralizing treatment
In the glyceryl monostearate crude product of step 1), add phosphoric acid, regulating pH is 6.0, stir 15 minutes, and deslagging after standing 2 hours then, filtrate is the thick ester of glyceryl monostearate.
3) one-level distillation
By step 2) in the thick ester feed liquid of glyceryl monostearate distill, distillation condition is as follows: temperature is 160 ℃, vacuum 150pa, thermal oil pressure 0.25-0.3MPA.Till steaming extremely steams without cut.
This step is steamed except the moisture in feed liquid.
4) secondary distillation
By steaming in step 3) except the feed liquid of moisture, carry out second stage distillation, steam except most extraction glycerine and free hydrogenated palm kernel oil.
Distillation condition is: temperature is 190 ℃, vacuum 3pa, thermal oil pressure 0.25-0.3MPA.Steaming obtains secondary distillation feed liquid till extremely steaming without cut.
5) three-stage distillation
Secondary distillation feed liquid in step 4) is entered to three-stage distillation, extract micro-glycerine and free hydrogenated palm kernel oil.
Distillation condition is: temperature is 200 ℃, vacuum 3pa, thermal oil pressure 0.25-0.3MPA.Steaming obtains three-stage distillation feed liquid till extremely steaming without cut.
6) level Four distillation:
Three-stage distillation feed liquid in step 5) is entered to level Four distillation, and separated glyceryl monostearate and stearic acid two glyceryl ester, glycerol stearate, obtain high-quality glyceryl monostearate.
Distillation condition is: temperature is 210 ℃, vacuum 0.1-7pa, and thermal oil pressure 0.25-0.3MPA, obtains glyceryl monostearate liquid.
7) glyceryl monostearate liquid spray is cooling, pack to obtain glyceryl monostearate finished product.
The quality examination result of finished product is:
Iodine number (gI
2/ 100g)≤2.0; Acid number (mg KOH/g): 1.0; Zero pour: 65.6 ℃; Saponification value (mg KOH/g): 165.Glyceryl monostearate content 99.20%.
embodiment 2
Prepare high-quality glyceryl monostearate, concrete technology is as follows:
1) preparation of glyceryl monostearate crude product
The preparation of step 1) glyceryl monostearate crude product:
First, 128kg glycerine is joined in esterification reaction tank, then 0.5kg sodium hydroxide slowly joins in esterification reaction tank, then is warming up to 90 degrees Celsius, stirs 30 minutes;
Secondly, 500kg hydrogenated liquid plam oil is joined in above-mentioned esterification reaction tank, be fully uniformly mixed, be warmed up to T
0be 215 ℃, control pressure P is-0.07Mpa, carries out esterification 30min, obtains glyceryl monostearate crude product;
2) neutralizing treatment
In the glyceryl monostearate crude product of step 1), add phosphoric acid, regulating pH is 6.5, stir 15 minutes, and deslagging after standing 2 hours then, filtrate is the thick ester of glyceryl monostearate.
3) one-level distillation
By step 2) in the feed liquid of having removed dregs distill, distillation condition is as follows: temperature is 170 ℃, vacuum 160pa, thermal oil pressure 0.25-0.3MPA.Till steaming extremely steams without cut.
This step is steamed except the moisture in feed liquid.
4) secondary distillation
By steaming in step 3) except the feed liquid of moisture, carry out second stage distillation, steam except most extraction glycerine and free hydrogenated palm kernel oil.
Distillation condition is: temperature is 200 ℃, vacuum 5pa, thermal oil pressure 0.25-0.3MPA.Till steaming extremely steams without cut.
5) three-stage distillation
By steaming in step 4), enter three-stage distillation except most of glycerine and the palmitic feed liquid of free hydrogenation, extract micro-glycerine and free hydrogenated palm kernel oil.
Distillation condition is: temperature is 210 ℃, vacuum 5pa, thermal oil pressure 0.25-0.3MPA.Steaming obtains three-stage distillation feed liquid till extremely steaming without cut.
6) level Four distillation:
Three-stage distillation feed liquid in step 5) is entered to level Four distillation, and separated glyceryl monostearate and stearic acid two glyceryl ester, glycerol stearate, obtain high-quality glyceryl monostearate.
Distillation condition is: temperature is 215 ℃, vacuum 0.1pa, and thermal oil pressure 0.25-0.3MPA, obtains glyceryl monostearate liquid.
7) glyceryl monostearate liquid spray is cooling, pack to obtain glyceryl monostearate finished product.
The quality examination result of finished product is:
Iodine number (gI
2/ 100g): 0.9; Acid number (mg KOH/g): 0.6; Zero pour: 65.6 ℃; Saponification value (mg KOH/g): 168.Glyceryl monostearate content 99.60%
embodiment 3
Prepare high-quality glyceryl monostearate, concrete technology is as follows:
1) preparation of glyceryl monostearate crude product
The preparation of step 1) glyceryl monostearate crude product:
First, 135kg glycerine is joined in esterification reaction tank, then 0.37kg sodium hydroxide slowly joins in esterification reaction tank, then is warming up to 90 degrees Celsius, stirs 30 minutes;
Secondly, 500kg hydrogenated liquid plam oil is joined in above-mentioned esterification reaction tank, be fully uniformly mixed, be warmed up to T
0be 218 ℃, control pressure P is-0.08Mpa, carries out esterification 30min, obtains glyceryl monostearate crude product;
2) neutralizing treatment
In the glyceryl monostearate crude product of step 1), add phosphoric acid, regulating pH is 7.0, stir 15 minutes, and deslagging after standing 2 hours then, filtrate is the thick ester of glyceryl monostearate.
3) one-level distillation
By step 2) in the feed liquid of having removed dregs distill, distillation condition is as follows: temperature is 170 ℃, vacuum 200pa, thermal oil pressure 0.25-0.3MPA.Till steaming extremely steams without cut.
This step is steamed except the moisture in feed liquid.
4) secondary distillation
By steaming in step 3) except the feed liquid of moisture, carry out second stage distillation, steam except most extraction glycerine and free hydrogenated palm kernel oil.
Distillation condition is: temperature is 195 ℃, vacuum 10pa, thermal oil pressure 0.25-0.3MPA.Till steaming extremely steams without cut.
5) three-stage distillation
By steaming in step 4), enter three-stage distillation except most of glycerine and the palmitic feed liquid of free hydrogenation, extract micro-glycerine and free hydrogenated palm kernel oil.
Distillation condition is: temperature is 210 ℃, vacuum 8pa, thermal oil pressure 0.25-0.3MPA.Steaming obtains three-stage distillation feed liquid till extremely steaming without cut.
6) level Four distillation:
Three-stage distillation feed liquid in step 5) is entered to level Four distillation, and separated glyceryl monostearate and stearic acid two glyceryl ester, glycerol stearate, obtain high-quality glyceryl monostearate.
Distillation condition is: temperature is 215 ℃, vacuum 0.1pa, and thermal oil pressure 0.25-0.3MPA, obtains glyceryl monostearate liquid.
7) glyceryl monostearate liquid spray is cooling, pack to obtain glyceryl monostearate finished product.
The quality examination result of finished product is:
Iodine number (gI
2/ 100g): 0.8; Acid number (mg KOH/g): 0.25; Zero pour: 65.7 ℃; Saponification value (mg KOH/g): 168.Glyceryl monostearate content 99.99%.
embodiment 4
Prepare high-quality glyceryl monostearate, concrete technology is as follows:
1) preparation of glyceryl monostearate crude product
The preparation of step 1) glyceryl monostearate crude product:
First, 141kg glycerine is joined in esterification reaction tank, then 0.4kg sodium hydroxide slowly joins in esterification reaction tank, then is warming up to 90 degrees Celsius, stirs 30 minutes;
Secondly, 500kg hydrogenated liquid plam oil is joined in above-mentioned esterification reaction tank, be fully uniformly mixed, be warmed up to T
0be 218 ℃, control pressure P is-0.08Mpa, carries out esterification 30min, obtains glyceryl monostearate crude product;
2) neutralizing treatment
Glyceryl monostearate crude product to step 1) adds phosphoric acid, and regulating pH is 7.0, stir 15 minutes, and deslagging after standing 2 hours then, filtrate is the thick ester of glyceryl monostearate.
3) one-level distillation
By step 2) in the feed liquid of having removed dregs distill, distillation condition is as follows: temperature is 180 ℃, vacuum 180pa, thermal oil pressure 0.25-0.3MPA.Till steaming extremely steams without cut.
This step is steamed except the moisture in feed liquid.
4) secondary distillation
By steaming in step 3) except the feed liquid of moisture, carry out second stage distillation, steam except most extraction glycerine and free hydrogenated palm kernel oil.
Distillation condition is: temperature is 195 ℃, vacuum 10pa, thermal oil pressure 0.25-0.3MPA.Till steaming extremely steams without cut.
5) three-stage distillation
By steaming in step 4), enter three-stage distillation except most of glycerine and the palmitic feed liquid of free hydrogenation, extract micro-glycerine and free hydrogenated palm kernel oil.
Distillation condition is: temperature is 210 ℃, vacuum 8pa, thermal oil pressure 0.25-0.3MPA.Steaming obtains three-stage distillation feed liquid till extremely steaming without cut.
6) level Four distillation:
Three-stage distillation feed liquid in step 5) is entered to level Four distillation, and separated glyceryl monostearate and stearic acid two glyceryl ester, glycerol stearate, obtain high-quality glyceryl monostearate.
Distillation condition is: temperature is 215 ℃, vacuum 0.1pa, and thermal oil pressure 0.25-0.3MPA, obtains glyceryl monostearate liquid.
7) glyceryl monostearate liquid spray is cooling, pack to obtain glyceryl monostearate finished product.
The quality examination result of finished product is:
Iodine number (gI
2/ 100g): 0.8; Acid number (mg KOH/g): 0.4; Zero pour: 65.7 ℃; Saponification value (mg KOH/g): 166.Glyceryl monostearate content 99.70%.
embodiment 5
Prepare high-quality glyceryl monostearate, concrete technology is as follows:
1) preparation of glyceryl monostearate crude product
The preparation of step 1) glyceryl monostearate crude product:
First, 154kg glycerine is joined in esterification reaction tank, then 0.3kg sodium hydroxide slowly joins in esterification reaction tank, then is warming up to 90 degrees Celsius, stirs 30 minutes;
Secondly, 500kg hydrogenated liquid plam oil is joined in above-mentioned esterification reaction tank, be fully uniformly mixed, be warmed up to T
0be 218 ℃, control pressure P is-0.08Mpa, carries out esterification 30min, obtains glyceryl monostearate crude product;
2) neutralizing treatment
Glyceryl monostearate crude product to step 1) adds phosphoric acid, and regulating pH is 7.0, stir 15 minutes, and deslagging after standing 2 hours then, filtrate is the thick ester of glyceryl monostearate.
3) one-level distillation
By step 2) in the feed liquid of having removed dregs distill, distillation condition is as follows: temperature is 200 ℃, vacuum 190pa, thermal oil pressure 0.25-0.3MPA.Till steaming extremely steams without cut.
This step is steamed except the moisture in feed liquid.
4) secondary distillation
By steaming in step 3) except the feed liquid of moisture, carry out second stage distillation, steam except most extraction glycerine and free hydrogenated palm kernel oil.
Distillation condition is: temperature is 210 ℃, vacuum 10pa, thermal oil pressure 0.25-0.3MPA.Till steaming extremely steams without cut.
5) three-stage distillation
By steaming in step 4), enter three-stage distillation except most of glycerine and the palmitic feed liquid of free hydrogenation, extract micro-glycerine and free hydrogenated palm kernel oil.
Distillation condition is: temperature is 210 ℃, vacuum 10pa, thermal oil pressure 0.25-0.3MPA.Steaming obtains three-stage distillation feed liquid till extremely steaming without cut.
6) level Four distillation:
Three-stage distillation feed liquid in step 5) is entered to level Four distillation, and separated glyceryl monostearate and stearic acid two glyceryl ester, glycerol stearate, obtain high-quality glyceryl monostearate.
Distillation condition is: temperature is 220 ℃, vacuum 5pa, and thermal oil pressure 0.25-0.3MPA, obtains glyceryl monostearate liquid.
7) glyceryl monostearate liquid spray is cooling, pack to obtain glyceryl monostearate finished product.
The quality examination result of finished product is:
Iodine number (gI
2/ 100g): 0.9; Acid number (mg KOH/g): 0.5; Zero pour: 66 ℃; Saponification value (mg KOH/g): 168.Glyceryl monostearate content 99.30%.
embodiment 6
Prepare high-quality glyceryl monostearate, concrete technology is as follows:
1) preparation of glyceryl monostearate crude product
The preparation of step 1) glyceryl monostearate crude product:
First, 166kg glycerine is joined in esterification reaction tank, then 0.2kg sodium hydroxide slowly joins in esterification reaction tank, then is warming up to 90 degrees Celsius, stirs 30 minutes;
Secondly, 500kg hydrogenated liquid plam oil is joined in above-mentioned esterification reaction tank, be fully uniformly mixed, be warmed up to T
0be 220 ℃, control pressure P is-0.08Mpa, carries out esterification 30min, obtains glyceryl monostearate crude product;
2) neutralizing treatment
In the glyceryl monostearate crude product of step 1), add phosphoric acid, regulating pH is 7.5, stir 15 minutes, and deslagging after standing 2 hours then, filtrate is the thick ester of glyceryl monostearate.
3) one-level distillation
By step 2) in the feed liquid of having removed dregs distill, distillation condition is as follows: temperature is 225 ℃, vacuum 170pa, thermal oil pressure 0.25-0.3MPA.Till steaming extremely steams without cut.
This step is steamed except the moisture in feed liquid.
4) secondary distillation
By steaming in step 3) except the feed liquid of moisture, carry out second stage distillation, steam except most extraction glycerine and free hydrogenated palm kernel oil.
Distillation condition is: temperature is 220 ℃, vacuum 10pa, thermal oil pressure 0.25-0.3MPA.Till steaming extremely steams without cut.
5) three-stage distillation
By steaming in step 4), enter three-stage distillation except most of glycerine and the palmitic feed liquid of free hydrogenation, extract micro-glycerine and free hydrogenated palm kernel oil.
Distillation condition is: temperature is 220 ℃, vacuum 8pa, thermal oil pressure 0.25-0.3MPA.Steaming obtains three-stage distillation feed liquid till extremely steaming without cut.
6) level Four distillation:
Three-stage distillation feed liquid in step 5) is entered to level Four distillation, and separated glyceryl monostearate and stearic acid two glyceryl ester, glycerol stearate, obtain high-quality glyceryl monostearate.
Distillation condition is: temperature is 230 ℃, vacuum 7pa, and thermal oil pressure 0.25-0.3MPA, obtains glyceryl monostearate liquid.
7) glyceryl monostearate liquid spray is cooling, pack to obtain glyceryl monostearate finished product.
The quality examination result of finished product is:
Iodine number (gI
2/ 100g): 1.0; Acid number (mg KOH/g): 0.8; Zero pour: 63-66 ℃; Saponification value (mg KOH/g): 165.Glyceryl monostearate content 99.10%.
Claims (1)
1. a preparation method for high quality glyceryl monostearate, comprises the steps:
The preparation of step 1) glyceryl monostearate crude product:
First, 135kg glycerine is joined in esterification reaction tank, then 0.37kg sodium hydroxide is slowly joined in esterification reaction tank, then be warming up to 90 degrees Celsius, stir 30 minutes;
Next, join 500kg hydrogenated liquid plam oil in above-mentioned esterification reaction tank, is fully uniformly mixed, and is warmed up to T0 and is
218 ℃, control pressure P is-0.08Mpa, carries out esterification 30min, obtains glyceryl monostearate crude product;
Step 2) neutralizing treatment
In above-mentioned reacted glyceryl monostearate crude product, add phosphoric acid, regulating pH is 7.0, stir 15 minutes, and deslagging after standing 2 hours then, filtrate is the thick ester of glyceryl monostearate;
The distillation of step 3) one-level
By step 2) in the thick ester of glyceryl monostearate distill, distillation condition is: temperature T 1 is 170 ℃, vacuum P1 is 200pa, thermal oil pressure 0.25-0.3Mpa steams to till steaming without cut, obtains one-level distillation feed liquid;
Step 4) secondary distillation
One-level distillation feed liquid in step 3) is carried out to second stage distillation, and distillation condition is: temperature T 2 is 195 ℃, and vacuum P2 is 10pa, and thermal oil pressure 0.25-0.3Mpa, obtains secondary distillation feed liquid;
Step 5) three-stage distillation
Secondary distillation feed liquid in step 4) is carried out to three-stage distillation, and distillation condition is: temperature T 3 is 210 ℃, and vacuum P3 is 8pa, and thermal oil pressure 0.25-0.3Mpa, obtains three-stage distillation feed liquid;
The distillation of step 6) level Four
Three-stage distillation feed liquid in step 5) is entered to level Four distillation, and distillation condition is: temperature T 4 is 215 ℃, and vacuum P4 is 0.1pa, and thermal oil pressure 0.25-0.3Mpa, obtains glyceryl monostearate liquid;
Step 7) is cooling by glyceryl monostearate liquid spray, packs to obtain glyceryl monostearate finished product;
Described high quality glyceryl monostearate is that the quality examination result of finished product is:
Iodine number gI
2/ 100g:0.8; Acid number mg KOH/g:0.25; Zero pour: 65.7 ℃; Saponification value mg KOH/g:168, glyceryl monostearate content 99.99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210501481.5A CN102964245B (en) | 2012-11-28 | 2012-11-28 | Preparation method of high-quality glycerin monostearate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210501481.5A CN102964245B (en) | 2012-11-28 | 2012-11-28 | Preparation method of high-quality glycerin monostearate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102964245A CN102964245A (en) | 2013-03-13 |
| CN102964245B true CN102964245B (en) | 2014-04-09 |
Family
ID=47794713
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210501481.5A Active CN102964245B (en) | 2012-11-28 | 2012-11-28 | Preparation method of high-quality glycerin monostearate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102964245B (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104177649A (en) * | 2014-08-06 | 2014-12-03 | 河南正通化工有限公司 | Polyglycerol fatty acid ester plasticizer and preparation method thereof |
| CN104489426B (en) * | 2014-11-28 | 2018-03-13 | 广州嘉德乐生化科技有限公司 | A kind of composition for food emulsification and preparation method thereof |
| CN104513491B (en) * | 2014-12-02 | 2016-10-05 | 广州市义和化工有限公司 | Anti-shrinkage agent for plastic processing and preparation method thereof |
| CN105152929B (en) * | 2015-08-05 | 2017-11-14 | 广州嘉德乐生化科技有限公司 | A kind of propylene glycol monostearate and its industrial process and application |
| CN106365988B (en) * | 2016-08-27 | 2019-04-26 | 广州嘉德乐生化科技有限公司 | A kind of preparation method of polyglycerol ester |
| CN107917971B (en) * | 2017-11-02 | 2020-11-24 | 苏州大学附属第一医院 | Application of myristic acid and glycerol composition in evaluating curative effect of chronic myelogenous leukemia TKI |
| CN108277090B (en) * | 2018-01-30 | 2019-04-05 | 浙江工业大学 | A kind of preparation method of low-sulphur biodiesel |
| CN108360249A (en) * | 2018-02-07 | 2018-08-03 | 枣庄市书源笔业有限公司 | A kind of multi-process writing brush sofening treatment technique |
| CN109896954A (en) * | 2019-03-27 | 2019-06-18 | 佳力士添加剂（海安）有限公司 | A kind of synthetic method of monopalmitin |
| CN111499509A (en) * | 2020-04-09 | 2020-08-07 | 佳格食品(中国)有限公司 | Production process of high-purity monoglyceride |
| CN111548270A (en) * | 2020-05-09 | 2020-08-18 | 上海早苗食品有限公司 | Molecular distillation glycerin monostearate emulsifier and preparation method thereof |
| CN113416132A (en) * | 2021-08-06 | 2021-09-21 | 杭州富春食品添加剂有限公司 | Production process for distilling low-glycerol glycerin monostearate |
| CN114231571B (en) * | 2021-12-29 | 2024-02-06 | 赞宇科技集团股份有限公司 | Production method for synthesizing monoglyceride stearate by immobilized composite lipase catalysis |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1076187A (en) * | 1993-01-19 | 1993-09-15 | 周端午 | The preparation method of high-purity monostearin |
| CN101575285B (en) * | 2009-04-29 | 2013-07-17 | 李普选 | Technical method for continuously producing fatty glyceride and special equipment thereof |
| CN101724508A (en) * | 2009-10-30 | 2010-06-09 | 华南理工大学 | Method for preparing monoglyceride by utilizing circulating esterification reaction and molecular distillation of diester |
| CN102241586B (en) * | 2011-05-12 | 2014-04-09 | 暨南大学 | Method for synthesizing and purifying high-purity fatty acyl monoglyceride |
| CN202398129U (en) * | 2012-01-12 | 2012-08-29 | 广州嘉德乐生化科技有限公司 | Internal rotor of evaporator for preparing molecular distillation glyceryl monostearate |
-
2012
- 2012-11-28 CN CN201210501481.5A patent/CN102964245B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN102964245A (en) | 2013-03-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102964245B (en) | Preparation method of high-quality glycerin monostearate | |
| CN103880672B (en) | High-purity DHA algae oil ethyl ester and be converted into the preparation method of glyceride | |
| CN105483170A (en) | Method for synthesizing Sn-2-monoglyceride through enzymic method | |
| CN107445826A (en) | A kind of preparation method of neural acid esters | |
| CN104370860A (en) | Diepoxide vegetable oil acid acetyl glyceride and synthesis method and application thereof | |
| CN108912195A (en) | A method of extracting phytosterol from cottonseed acidification oil | |
| CN108265089B (en) | Oil and fat composition containing 1, 3-dioleoyl-2-palmitic acid triglyceride and preparation method thereof | |
| CN101880601A (en) | Method for preparing linoleic acid from idesia polycarpa Maxium. Var. vestita Diels oil | |
| CN102993009B (en) | Preparation method of glycerin monostearate alpha crystal | |
| CN107254494A (en) | A kind of glycerine ester type PUFA preparation method | |
| CN103937616A (en) | Method for extracting high-purity unsaturated fatty acid from soybean oil | |
| CN109666533A (en) | Refined horse oil and its refining extracting method and application | |
| CN204058300U (en) | A kind of high-temperature reflux hydrolysate oil is separated the device preparing glycerine | |
| CN105418699A (en) | Method and production device for continuously producing alkyl glucoside | |
| CN108558700A (en) | A kind of synthetic method of 1,2- pentanediols | |
| CN102942995B (en) | Method for separating and modifying plant oil | |
| CN109535104B (en) | A kind of production method of epoxidized soybean oil | |
| CN106565454A (en) | Preparation method for conjugated linoleic acid | |
| CN102838449A (en) | Method for producing octacosanol with special content | |
| CN114920642A (en) | Separation process for obtaining high-purity fatty acid monoglyceride and fatty acid diglyceride | |
| CN113881717A (en) | Preparation method of structural grease and structural grease prepared by same | |
| CN104531362A (en) | Method for preparing tripolyglycerol fatty acid ester by solid superacid catalysis | |
| CN113512568A (en) | Preparation method of linoleic acid-rich structural grease | |
| CN114163326A (en) | Preparation method of structural grease and structural grease prepared by same | |
| CN105132153A (en) | Method for preparing squid liver oil |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: 510000 No. 6 Huafeng Road, Yonghe District, Guangzhou Economic and Technological Development Zone, Guangdong Province Patentee after: Guangdong Jiadele Technology Co.,Ltd. Address before: No. 6 Huafeng Road, Yonghe Avenue, Guangzhou Economic and Technological Development Zone, Guangdong Province, 510530 Patentee before: GUANGZHOU CARDLO BIOCHEMICAL TECHNOLOGY Co.,Ltd. |
|
| CP03 | Change of name, title or address |