CN106084209B - A kind of production technology of polyglyceryl fatty acid ester - Google Patents
A kind of production technology of polyglyceryl fatty acid ester Download PDFInfo
- Publication number
- CN106084209B CN106084209B CN201610583635.8A CN201610583635A CN106084209B CN 106084209 B CN106084209 B CN 106084209B CN 201610583635 A CN201610583635 A CN 201610583635A CN 106084209 B CN106084209 B CN 106084209B
- Authority
- CN
- China
- Prior art keywords
- vacuum degree
- reaction kettle
- fatty acid
- catalyst
- acid ester
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
- C08G65/48—Polymers modified by chemical after-treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2650/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G2650/28—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type
- C08G2650/38—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type containing oxygen in addition to the ether group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2650/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G2650/28—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type
- C08G2650/52—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type obtained by dehydration of polyhydric alcohols
- C08G2650/54—Polyglycerols
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Medicinal Preparation (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention relates to a kind of production technologies of polyglyceryl fatty acid ester, belong to emulsifier preparation field.It is an object of the invention to overcome prior art defect, a kind of production technology of polyglyceryl fatty acid ester is provided, in the technique polyglyceryl fatty acid ester of high quality is synthesized by reasonably selecting catalyst and two-phase method, the method reaction condition is mildly easy to control, product color is obviously improved, without peculiar smell, impurity is fewer, rational in infrastructure, function admirable, and environmentally friendly, three-waste free discharge.
Description
Technical field
The present invention relates to a kind of production technologies of polyglyceryl fatty acid ester, belong to emulsifier preparation field.
Background technology
Polyglyceryl fatty acid ester is nonionic surfactant, abbreviation PGFE, and polyglycerol ester has hydrophilic, the dual spy of oleophylic concurrently
Property, there is higher HLB value, with the multiple performances such as good emulsification, scattered, moistening, stable, blistering, be soluble in grease, ethyl alcohol
And organic solvent, it can be scattered in hot water.The decomposable asymmetric choice net during body metabolism so as to participate in being metabolized, is immediately used by the body, has
Tight security is a kind of highly effective and safe additive, recommends to make by FAO (Food and Agriculture Organization of the United Nation) and the World Health Organization (FAO/WHO)
With.Polyglycerol ester quite stable, chance salt content in acid, alkalescence and neutral environment also has fine emulsibility when higher simultaneously.
Polyglycerol ester is colourless, it is tasteless, be not susceptible to hydrolyze, have no adverse effects to product appearance, smell；It can be answered with other emulsifiers
Match somebody with somebody, there is good synergistic function, thus be widely used in food, daily use chemicals, oil, weaving, coating, plastics, pesticide, rubber
Glue, medicine and other fields.Polyglycerol ester has become a kind of nonionic surfactant rapidly developed.
A kind of method that CN103172851A and gutter oil prepare polyglyceryl fatty acid ester.This method first to gutter oil into
Row pretreatment, and pretreated gutter oil and water are sent into hydrolytic reaction pot, gutter oil is made to be issued in high temperature, acid condition
Raw hydrolysis, obtains aliphatic acid, water vapour, crude glycerine and grease；Gained aliphatic acid and water vapour after condensing reflux, then
Distillation removal water vapour, obtains fatty acid product；Gained crude glycerine by separation, centrifugation purification and it is refined finally obtain it is refined sweet
Oil, refined glycerine obtain polyglycereol using polymerisation, and most polyglycereol and aliphatic acid are sent into reaction kettle of the esterification at last, make it
Esterification occurs under high temperature, alkaline condition, obtains polyglyceryl fatty acid ester product.The polyglycerol ester that this method is prepared
Although fat acid esters realizes the recycling of discarded object, but final products is of low quality, it is difficult to meet existing demand.
CN104177649A discloses a kind of polyglycerol ester plasticizer and preparation method thereof, belongs to field of plastics additives.This hair
It is bright to make the not only ester group containing polarized, while the also ehter bond containing low pole in plasticizer molecule by introducing ehter bond, so that
Glass transition temperature of polymer reduces, and improves heat-resisting cold tolerance.
CN1308276C is to generate gathering containing cyclic structure for cyclic structure when sloughing hydrone on having in the molecule
The polyglycereol significantly reduced there are ratio of glycerine and on the polyglyceryl fatty acid ester with excellent surface activity.For 1
Mole of glycerin gradually adds both 2 moles or 2 moles or more glycidol and catalyst and is allowed to react, obtained glycerine,
According to the obtained intensity ratio of liquid chromatography/mass analysis, polyglycereol (1) adds up to: the polyglycereol (2) containing cyclic structure
Total=70% or more than 70%: 30% or less than 30% (the total of the two is 100 weight %), average degree of polymerization<n>For 2
Or more than 2.The polyglycereol is made to can obtain corresponding polyglyceryl fatty acid ester with the reaction of aliphatic acid.
The manufacturing technology of existing polyglyceryl fatty acid ester product is not perfect in the market, and product quality is bad, generally existing color
Pool compared with it is deep, have peculiar smell, emulsifying ability be low, impurity mostly with production cost it is high the problems such as, limit it in foods and cosmetics
Application.
The content of the invention
It is an object of the invention to overcome prior art defect, a kind of production technology of polyglyceryl fatty acid ester is provided, it should
Method reaction condition is mildly easy to control, product color is obviously improved, without peculiar smell, impurity is fewer, rational in infrastructure, function admirable,
And environmentally friendly, three-waste free discharge.
The present invention is achieved through the following technical solutions above-mentioned technical purpose：
A kind of production method of polyglyceryl fatty acid ester, specifically includes following steps：
1) glycerine of precise is pumped into reaction kettle, opens heating unit and agitating device, control material temperature is 65
℃-95℃；The catalyst of 1/3 amount is slowly added into reaction kettle and is passed through nitrogen, it is 0.01- to control the vacuum degree in reaction kettle
0.03MPa progressively heats up material in reactor temperature being raised to 200-280 DEG C, and control vacuum degree is in 0.02-0.09Mpa, heat preservation
Stirring 90-180 minutes；Stop heating after the completion of heat preservation and open cooling water valve, vacuum degree is adjusted to 0.03Mpa, is protected in nitrogen
Under, temperature of charge is down to 100 DEG C -120 DEG C, emptying eliminates negative pressure, sampling detection；
2) stearic acid is pumped into reaction kettle, opens agitating device, the catalyst of remaining 2/3 amount is added in reaction kettle；
Vacuum is opened, vacuum degree is controlled to be warming up to 130-160 DEG C, insulated and stirred 20-50 minutes for 0.02-0.05MPa；Continue to heat up
To 175-195 DEG C, vacuum degree control is in 0.06-0.09MPa, insulated and stirred 110-210 minutes；
3) diatomite is added in into reaction kettle, under nitrogen protection, vacuum degree 0.03Mpa, after stirring 20-50 minutes, into
Filter press filtering after dust to get.
In the production method of polyglyceryl fatty acid ester described above, the catalyst amount is the 1%- of qualities of glycerin
1.5%.The catalyst is sodium hydroxide and the compound of calcium hydroxide.Sodium hydroxide and hydrogen in the wherein described compound
The molar ratio of calcium oxide is 1:0.5-0.9, it is preferable that the molar ratio of sodium hydroxide and calcium hydroxide is 1 in the compound:
0.7, at this time the reaction speed of polymerisation faster, reaction condition milder.
Glycerine and stearic mass ratio are 1 in the production method of polyglyceryl fatty acid ester described above：0.6-1.4,
Preferably, the glycerine and stearic mass ratio 1:1.
In the production method of polyglyceryl fatty acid ester described above, glycerine is 1 with diatomaceous mass ratio:0.01-
0.05。
As can be seen from Table 1, the present invention complies fully with the index listed by quality standard compared with quality standard, and
It is higher than quality standard in terms of content of beary metal and sulfated ass.And although polyglycerol fatty acid has then been prepared in comparative example 1
Ester production, but its sulfated ass, fusing point and content of beary metal are not up to the index of quality standard, this shows that its quality is not so good as this hair
It is bright.2 process conditions of comparative example are similar, but its catalyst and lack two sections of building-up processes in building-up process in reaction condition,
Its quality does not reach quality standards.This shows that the process conditions that the present invention is controlled generate unexpected technique effect.
Compared with prior art, the present invention the technique effect of acquired protrusion is：
1) reaction condition of the present invention is mildly easy to control, has selected suitable preparation process, by the polymerization for changing polyglycereol
Degree, esterification degree and esterified positions, can prepare the polyglycerol ester of different structure, and product color is obviously improved, without peculiar smell, impurity
Fewer, rational in infrastructure, function admirable, and environmentally friendly, three-waste free discharge.
2) for the present invention using negative pressure of vacuum reaction process, reaction temperature is 30-50 DEG C lower than traditional handicraft, has saved a large amount of energy
Source；Using diatomite decoloration process, color and luster is obviously improved, and also adsorbable other impurity, avoid the residual after hydrogen peroxide bleaching
And side effect.
3) the preparation-obtained polyglyceryl fatty acid ester quality of the present invention is higher, can be used not only in food, medicine, cosmetics
Field, it is also possible to which in weaving, coating, plastics, pesticide, rubber materials, market potential is very big.
Specific embodiment
The present invention is further described below by way of specific embodiment, but the embodiment does not limit this hair in any way
The protection domain of bright patent.
A kind of production method of 1 polyglyceryl fatty acid ester of embodiment
Stock：Glycerine 900kg, stearic acid 1000kg, catalyst 12.5kg.The wherein described catalyst for sodium hydroxide and
The compound of calcium hydroxide, molar ratio 1：0.5.
The preparation method of the polyglycerol ester includes the following steps：
1. the glycerine of precise is pumped into reaction kettle, heating unit and agitating device are opened, control material temperature is 80
DEG C or so；The catalyst that 1/3 amount is slowly added into reaction kettle is passed through nitrogen, and opening water-circulating pump, (vacuum degree control exists
0.01MPa), progressively heat up；Temperature of charge is raised to 220-240 DEG C, control vacuum degree in 0.07Mpa, divide by insulated and stirred 150
Clock；Stop heating, open cooling water valve, vacuum degree is adjusted to 0.03Mpa, under nitrogen protection, temperature of charge is down to 100 DEG C
When, emptying eliminates negative pressure, sampling detection.
2. the stearic acid measured is pumped into reaction kettle, agitating device is opened, the catalyst of remaining 2/3 amount is added in
In reaction kettle；Vacuum is opened, vacuum degree is controlled to be warming up to 150 DEG C, insulated and stirred 40 minutes for 0.02-0.05MPa；After of continuing rising
Temperature is to 190 DEG C, and vacuum degree control is in 0.07MPa, insulated and stirred 180 minutes；
3. adding in 20kg diatomite, under nitrogen protection, vacuum degree 0.03Mpa after stirring 30 minutes, is filtered into filter press
Afterwards, dust.
A kind of production method of 2 polyglyceryl fatty acid ester of embodiment
Stock：Glycerine 1200kg, stearic acid 1200kg, catalyst 14.5kg.The wherein described catalyst is sodium hydroxide
With the compound of calcium hydroxide, molar ratio 1：0.7.
The preparation method of the polyglycerol ester includes the following steps：
1. the glycerine of precise is pumped into reaction kettle, opens heating unit and agitating device, control material temperature exist
80 DEG C or so；The catalyst of 1/3 amount is slowly added into reaction kettle and is passed through nitrogen, opening water-circulating pump, (vacuum degree control exists
0.02MPa), progressively heat up；Temperature of charge is raised to 230-250 DEG C, control vacuum degree in 0.07Mpa, divide by insulated and stirred 180
Clock.Stop heating, open cooling water valve, vacuum degree is adjusted to 0.03Mpa, under nitrogen protection, temperature of charge is down to 100 DEG C
When, emptying eliminates negative pressure, sampling detection.
2. the stearic acid measured is pumped into reaction kettle, stirring is opened, the catalyst of remaining 2/3 amount is added in into reaction kettle
In；Vacuum is opened, vacuum degree is controlled to be warming up to 150 DEG C, insulated and stirred 50 minutes for 0.02-0.05MPa；It is continuously heating to 195
DEG C, vacuum degree control is in 0.09MPa, insulated and stirred 200 minutes；
3. adding in 25kg diatomite, under nitrogen protection, vacuum degree 0.03Mpa, stirring after forty minutes, is filtered into filter press
Afterwards, dust.
A kind of production method of 3 polyglyceryl fatty acid ester of embodiment
Stock：Glycerine 1400kg, stearic acid 1300Kg, catalyst 15.0kg.The wherein described catalyst is sodium hydroxide
With the compound of calcium hydroxide, molar ratio 1：0.9.
The preparation method of the polyglycerol ester includes the following steps：
1. the glycerine of precise is pumped into reaction kettle, opens heating unit and agitating device, control material temperature exist
80 DEG C or so；The catalyst that 1/3 amount is slowly added into reaction kettle is passed through nitrogen, and opening water-circulating pump, (vacuum degree control exists
0.03MPa), progressively heat up；Temperature of charge is raised to 240-260 DEG C, control vacuum degree in 0.06Mpa, divide by insulated and stirred 240
Clock.Stop heating, open cooling water valve, vacuum degree is adjusted to 0.03Mpa, under nitrogen protection, temperature of charge is down to 100 DEG C
When, emptying eliminates negative pressure, sampling detection.
2. the stearic acid measured is pumped into reaction kettle, stirring is opened, the catalyst of remaining 2/3 amount is added in into reaction kettle
In；Vacuum is opened, vacuum degree is controlled to be warming up to 160 DEG C, insulated and stirred 50 minutes for 0.03-0.05MPa；It is continuously heating to 190
DEG C, vacuum degree control is in 0.09MPa, insulated and stirred 180 minutes；
3. adding in 40kg diatomite, under nitrogen protection, vacuum degree 0.03Mpa after stirring 45 minutes, is filtered into filter press
Afterwards, dust.
A kind of production method of 4 polyglyceryl fatty acid ester of embodiment
Stock：Glycerine 1200kg, stearic acid 1300Kg, catalyst 14.0kg.The wherein described catalyst is sodium hydroxide
With the compound of calcium hydroxide, molar ratio 1：0.5.
The preparation method of the polyglycerol ester includes the following steps：
1. the glycerine of precise is pumped into reaction kettle, opens heating unit and agitating device, control material temperature exist
80 DEG C or so；The catalyst that 1/3 amount is slowly added into reaction kettle is passed through nitrogen, and opening water-circulating pump, (vacuum degree control exists
0.03MPa), progressively heat up；Temperature of charge is raised to 240-260 DEG C, control vacuum degree in 0.06Mpa, divide by insulated and stirred 240
Clock.Stop heating, open cooling water valve, vacuum degree is adjusted to 0.03Mpa, under nitrogen protection, temperature of charge is down to 100 DEG C
When, emptying eliminates negative pressure, sampling detection.
2. the stearic acid measured is pumped into reaction kettle, stirring is opened, the catalyst of remaining 2/3 amount is added in into reaction kettle
In；Vacuum is opened, vacuum degree is controlled to be warming up to 160 DEG C, insulated and stirred 50 minutes for 0.03-0.05MPa；It is continuously heating to 190
DEG C, vacuum degree control is in 0.09MPa, insulated and stirred 180 minutes；
3. adding in 40kg diatomite, under nitrogen protection, vacuum degree 0.03Mpa after stirring 45 minutes, is filtered into filter press
Afterwards, dust.
A kind of production method of 5 polyglyceryl fatty acid ester of embodiment
Stock：Glycerine 1400kg, stearic acid 1300kg, catalyst 15.0kg.The wherein described catalyst is sodium hydroxide
With the compound of calcium hydroxide, molar ratio 1：0.7.
The preparation method of the polyglycerol ester includes the following steps：
1. the glycerine of precise is pumped into reaction kettle, opens heating unit and agitating device, control material temperature exist
80 DEG C or so；The catalyst that 1/3 amount is slowly added into reaction kettle is passed through nitrogen, and opening water-circulating pump, (vacuum degree control exists
0.03MPa), progressively heat up；Temperature of charge is raised to 240-260 DEG C, control vacuum degree in 0.06Mpa, divide by insulated and stirred 240
Clock.Stop heating, open cooling water valve, vacuum degree is adjusted to 0.03Mpa, under nitrogen protection, temperature of charge is down to 100 DEG C
When, emptying eliminates negative pressure, sampling detection.
2. the stearic acid measured is pumped into reaction kettle, stirring is opened, the catalyst of remaining 2/3 amount is added in into reaction kettle
In；Vacuum is opened, vacuum degree is controlled to be warming up to 160 DEG C, insulated and stirred 50 minutes for 0.03-0.05MPa；It is continuously heating to 190
DEG C, vacuum degree control is in 0.09MPa, insulated and stirred 180 minutes；
3. adding in 40kg diatomite, under nitrogen protection, vacuum degree 0.03Mpa after stirring 45 minutes, is filtered into filter press
Afterwards, dust.
Comparative example 1 is prepared according to 2 the method for patent application CN 103172851A embodiments
(1), the gutter oil of 100 parts by weight is sent into preprocessor 1, first, the double of 3 parts by weight is added in into gutter oil
Oxygen water controls preprocessor temperature to continuously stir 20min for 60 DEG C, add the atlapulgite of 4 parts by weight, by preprocessor
70 DEG C are warming up to, then continuously stirs 20min and obtains pretreated gutter oil；
(2), the pretreated gutter oil being prepared in step (1) is sent into hydrolytic reaction pot 2, added thereto
The water of 80 parts by weight and the concentrated sulfuric acid that 1 parts by weight concentration is 98%, the concentrated sulfuric acid are catalyst, control hydrolytic reaction pot 2
Temperature is 200~250 DEG C, and pressure is normal pressure, makes gutter oil that hydrolysis, water occur with water vapour under high temperature, condition of normal pressure
Solution obtains aliphatic acid, water vapour, crude glycerine and grease；
(3), aliphatic acid obtained by (2) step is entered with water vapour in condenser 3, after conventional condensation, enters back into distillation
In device 4, the temperature that controls distiller 4 is 100~105 DEG C, pressure is normal pressure, separates to obtain fatty acid product and water；
(4), the separated water of (3) step is returned in the hydrolytic reaction pot 2 of (2) step, realizes recycling for water；
(5), the crude glycerine in the hydrolytic reaction pot 2 of (2) step and grease are subjected to stratification, control hydrolytic reaction pot
2 temperature is 60~80 DEG C, pressure is normal pressure, and it is crude glycerine product to collect lower floor's liquid；
(6), crude glycerine product obtained by (5) step is sent into centrifuge 5,15 weight is added in into the crude glycerine product
The methanol of part is diluted, and is centrifuged 15 minutes on centrifuge 5, and it is glycerol semi-final product to collect lower floor's liquid；
(7), glycerol semi-final product obtained by (6) step is moved into rectifier 6, the temperature for controlling rectifier 6 is 70 DEG C, normal pressure
Methanol is distilled to recover, 164~204 DEG C of fractions are collected in vacuum distillation, are refined glycerine；
(8), the methanol by the recycling of (7) step is returned in the centrifuge 5 of (6) step, realizes recycling for methanol；
(9), refined glycerine is added in polymerization reaction kettle 7, first, is passed through nitrogen, the temperature for controlling polymerization reaction kettle 7 is
It 120 DEG C~150 DEG C, preheating 10~30 minutes, then adds in the sodium hydroxide of 1 parts by weight, the sodium hydroxide is catalyst, and
It is stirred continuously, the temperature of polymerization reaction kettle 7 is risen to 220 DEG C~250 DEG C, when reaction 5~6 is small, obtains polyglycereol product；
(10), polyglycereol product obtained by (9) step is sent into reaction kettle of the esterification 8, adds in the sodium hydroxide of 1 parts by weight,
The sodium hydroxide is catalyst, and reaction kettle of the esterification 8 is warming up to 240 DEG C or so, by fatty acid product obtained by (3) step in batches
It is added in reaction kettle of the esterification 8, and is stirred continuously, the fatty acid product is interior when 1.5 is small to be added；To esterification in reaction process
Reaction kettle 8 is passed through the water vapour of nitrogen removal generation, and constantly analyzes acid value, and when acid value is less than 10, reaction was completed, after cooling
Collect final polyglyceryl fatty acid ester product.
Comparative example 2 prepares polyglyceryl fatty acid ester according to following techniques
Stock：Glycerine 1400kg, stearic acid 1300Kg, catalyst 15.0kg, wherein catalyst are sodium hydroxide.
The preparation method of the polyglycerol ester includes the following steps：
1. the glycerine of precise is pumped into reaction kettle, the catalyst that 1/3 amount is slowly added into reaction kettle is passed through nitrogen
Gas opens water-circulating pump (vacuum degree control is in 0.03MPa), progressively heats up；Temperature of charge is raised to 300 DEG C, controls vacuum degree
In 0.05Mpa, insulated and stirred 80 minutes.Stop heating, open cooling water valve, vacuum degree is adjusted to 0.03Mpa, is protected in nitrogen
Under, when temperature of charge is down to 100 DEG C, emptying eliminates negative pressure, sampling detection.
2. the stearic acid measured is pumped into reaction kettle, stirring and vacuum are opened；It is 0.03- to control vacuum degree
0.05MPa is warming up to 160 DEG C, insulated and stirred 230 minutes；
3. adding in 40kg diatomite, under nitrogen protection, vacuum degree 0.03Mpa after stirring 45 minutes, is filtered into filter press
Afterwards, dust.
Polyglyceryl fatty acid ester product will be made according to the preparation process described in embodiment 1- embodiments 5, measure its quality
Parameter is as shown in the table, concurrently sets comparative example 1 and comparative example 2 is used as reference.
As can be seen from Table 1, the present invention complies fully with the index listed by quality standard compared with quality standard, and
It is higher than quality standard in terms of content of beary metal and sulfated ass.And although polyglycerol fatty acid has then been prepared in comparative example 1
Ester production, but its sulfated ass, fusing point and content of beary metal are not up to the index of quality standard, this shows that its quality is not so good as this hair
It is bright.2 process conditions of comparative example are similar, but its catalyst and lack two sections of building-up processes in building-up process in reaction condition,
Its quality does not reach quality standards.This shows that the process conditions that the present invention is controlled generate unexpected technique effect.
Claims (2)
1. a kind of production method of polyglyceryl fatty acid ester, specifically includes following steps：
1）The glycerine of precise is pumped into reaction kettle, opens heating unit and agitating device, control material temperature is at 65 DEG C -95
℃；The catalyst of 1/3 amount is slowly added into reaction kettle and is passed through nitrogen, it is 0.01- to control the vacuum degree in reaction kettle
0.03MPa progressively heats up material in reactor temperature being raised to 200-280 DEG C, and control vacuum degree is in 0.02-0.09MPa, guarantor
Temperature stirring 90-180 minutes；Stop heating after the completion of heat preservation and open cooling water valve, vacuum degree is adjusted to 0.03MPa, is protected in nitrogen
Under shield, temperature of charge is down to 100 DEG C -120 DEG C, emptying eliminates negative pressure, sampling detection；
2）Stearic acid is pumped into reaction kettle, opens agitating device, the catalyst of remaining 2/3 amount is added in reaction kettle；It opens
Vacuum controls vacuum degree to be warming up to 130-160 DEG C, insulated and stirred 20-50 minutes for 0.02-0.05MPa；It is continuously heating to
175-195 DEG C, vacuum degree control is in 0.06-0.09MPa, insulated and stirred 110-210 minutes；
3）Diatomite is added in into reaction kettle, under nitrogen protection, vacuum degree 0.03MPa, after stirring 20-50 minutes, into press filtration
Machine filtering after dust to get；
The catalyst amount is the 1%-1.5% of qualities of glycerin, and the catalyst is answered for sodium hydroxide and calcium hydroxide
With object, the molar ratio of sodium hydroxide and calcium hydroxide is 1 in the compound:0.7, glycerine and stearic mass ratio are 1：
0.6-1.4, glycerine are 1 with diatomaceous mass ratio:0.01-0.05.
2. the production method of polyglyceryl fatty acid ester according to claim 1, which is characterized in that the glycerine and tristearin
The mass ratio 1 of acid:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610583635.8A CN106084209B (en) | 2016-07-22 | 2016-07-22 | A kind of production technology of polyglyceryl fatty acid ester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610583635.8A CN106084209B (en) | 2016-07-22 | 2016-07-22 | A kind of production technology of polyglyceryl fatty acid ester |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106084209A CN106084209A (en) | 2016-11-09 |
| CN106084209B true CN106084209B (en) | 2018-05-22 |
Family
ID=57449998
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610583635.8A Active CN106084209B (en) | 2016-07-22 | 2016-07-22 | A kind of production technology of polyglyceryl fatty acid ester |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106084209B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109762156A (en) * | 2018-12-29 | 2019-05-17 | 佛山市银美联合科技有限公司 | A kind of deodorizing methods in esters synthesis |
| CN113277945B (en) * | 2021-01-14 | 2022-03-29 | 郑州大河食品科技有限公司 | Polyglycerol fatty acid ester and preparation method thereof |
| CN113105621A (en) * | 2021-04-12 | 2021-07-13 | 郑州大河食品科技有限公司 | Method for improving emulsifying property of polyglycerol fatty acid ester |
| CN113912835B (en) * | 2021-11-26 | 2023-05-12 | 浙江金棕榈科技股份有限公司 | Polyglycerol fatty acid ester and preparation process thereof |
| CN114106852B (en) * | 2021-11-29 | 2023-08-01 | 广东广益科技实业有限公司 | Preparation method of powder cake emulsifying foaming agent |
| CN115109252A (en) * | 2022-06-16 | 2022-09-27 | 广州嘉德乐生化科技有限公司 | Preparation method of polyglycerol fatty acid ester for food processing |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786944A (en) * | 2010-01-11 | 2010-07-28 | 济南东润精化科技有限公司 | Preparation method of high-quality polyglycerol |
-
2016
- 2016-07-22 CN CN201610583635.8A patent/CN106084209B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786944A (en) * | 2010-01-11 | 2010-07-28 | 济南东润精化科技有限公司 | Preparation method of high-quality polyglycerol |
Non-Patent Citations (2)
| Title |
|---|
| "聚甘油脂肪酸酯合成及应用";周燕霞等;《粮食与油脂》;20081231(第7期);6-10 * |
| "聚甘油酯合成及特性研究";肖凯军等;《现代食品科技》;20081031;第24卷(第10期);966-968 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106084209A (en) | 2016-11-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106084209B (en) | A kind of production technology of polyglyceryl fatty acid ester | |
| MX2012000591A (en) | High temperature lignin separation process. | |
| JPS62111700A (en) | Recovery of glucose, lgnin and cellulose from lignocellulose plant stock material | |
| CN106755151B (en) | Method for producing ARA by utilizing microbial fermentation | |
| CN100376525C (en) | Method for refining glycerol being as byproduct of biology diesel oil | |
| CN110407950B (en) | Method for extracting intracellular polysaccharide of mould by using green solvent | |
| CN110894516A (en) | Method for preparing functional beef tallow by biological method | |
| CN108640966B (en) | Eutectic solvent for extracting tea saponin from tea seed meal and extraction process | |
| CN103382413B (en) | Refining process for reducing content of MCPD in tea seed oil | |
| CN106832050B (en) | The method of pectin is separated from Siraitia grosvenorii production waste residue | |
| US8759556B2 (en) | Method for obtaining a fraction enriched with functionalized fatty acid esters from seeds of oleaginous plants | |
| CN103254993A (en) | Rice bran crude oil separation method | |
| CN114097894A (en) | Low-cholesterol beef tallow and preparation method thereof | |
| CN105670800A (en) | Method for preparing fatty acid by utilizing illegal cooking oil | |
| CN117210971A (en) | Method for preparing high-water-holding capacity and high-oil-holding capacity nano citrus fiber | |
| CN104711112A (en) | Method for realization of combined production of high quality rice bran oil and ferulic acid from rice bran | |
| CN108018127A (en) | A kind of preparation method of unsaturation mono-fatty acid glyceride | |
| CN106365988B (en) | A kind of preparation method of polyglycerol ester | |
| CN115286727B (en) | Preparation method of low-residue polyvinyl butyral | |
| CN111548862A (en) | Self-aggregating aqueous phospholipid | |
| TW200846459A (en) | Additives for increasing the separation yield of tall oil soap from black liquors | |
| CN101412917A (en) | Method for preparing biodiesel | |
| CN104844442A (en) | Method for preparing mixed acid from solvent mother liquor | |
| CN113397206B (en) | Preparation method of carboxymethylated momordica grosvenori polysaccharide and application of carboxymethylated momordica grosvenori polysaccharide in tobacco humectant | |
| CN111484898B (en) | Yellow solid phospholipid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20221221 Address after: No. 6, Huafeng Road, Yonghe District, Guangzhou Economic and Technological Development Zone, Guangdong 510530 Patentee after: GUANGZHOU CARDLO BIOCHEMICAL TECHNOLOGY Co.,Ltd. Address before: Building 4, No. 6, Huafeng Road, Guangzhou High tech Development Zone, Guangdong 510070 Patentee before: GUANGZHOU HUANGLONG BIOTECHNOLOGY Co.,Ltd. |
|
| TR01 | Transfer of patent right | ||
| CP01 | Change in the name or title of a patent holder |
Address after: No. 6, Huafeng Road, Yonghe District, Guangzhou Economic and Technological Development Zone, Guangdong 510530 Patentee after: Guangdong Jiadele Technology Co.,Ltd. Address before: No. 6, Huafeng Road, Yonghe District, Guangzhou Economic and Technological Development Zone, Guangdong 510530 Patentee before: GUANGZHOU CARDLO BIOCHEMICAL TECHNOLOGY Co.,Ltd. |
|
| CP01 | Change in the name or title of a patent holder |