CN110724257A - Method for extracting polyglycerol from glycerol slag - Google Patents
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- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
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Abstract
The invention discloses a method for extracting polyglycerol from glycerol slag, which comprises the steps of treating the glycerol slag and rectifying a primary glycerol product, and specifically comprises the steps of mixing a prepared glycerol slag solution with a separating agent solution, heating and stirring, cooling, standing and separating into a supernatant and a lower emulsion, filtering to obtain the supernatant which is the primary glycerol product, and obtaining the lower emulsion which is a solid mixture of ester and phosphate; and then the obtained glycerin primary product is treated by a three-stage molecular distillation process to remove impurities such as free glycerin, ester compounds and the like, and the obtained distillation product is the polyglycerol. The method solves the problem of solid waste discharge of the bottom glycerin residue of the current molecular distillation monoglyceride manufacturer by the polyglycerol prepared from the waste glycerin residue, also solves the problems of industrial circulation and energy conservation and environmental protection of the molecular distillation industry, and the product prepared by the method has good quality and light color, and the content of the polyglycerol in the product is up to more than 95 percent.
Description
Technical Field
The invention relates to a method for extracting polyglycerol from glycerol residues, in particular to a method for extracting, separating and purifying polyglycerol from glycerol residues of molecular distillation monoglyceride and ester emulsifiers.
Background
Polyglycerols are important fine chemicals and synthetic intermediates. The polyglycerol ester synthesized by polyglycerol with different polymerization degrees and different fatty acids has the functions of emulsification, dispersion, corrosion prevention, lubrication, wetting and the like, and is mainly used as a humectant, a moisture absorbent, a lubricant, a softener, a thickener, a plasticizer, a diluent and an antifreezing agent to be applied to food, medicine, daily chemical and industrial surfactants. Because the polyglycerol must be synthesized before the polyglycerol ester is synthesized, the polyglycerol is synthesized by taking strong base as a catalyst at high temperature at present, and the polyglycerol synthesized by the method has the defects of high free glycerol content, deep color, high viscosity, large smell and the like. Meanwhile, the other problem is that a great amount of glycerin residues are generated in the distillation production of glycerin and the production process of molecular distillation monoglyceride and ester emulsifier, and the glycerin residues are rich in rich polyglycerol, so how to fully utilize the polyglycerol in the glycerin residues can change waste into valuable, save income and protect the environment, which becomes a problem to be solved urgently in modern society.
Currently, publication No. CN101104683A discloses a method for extracting polyglycerol from glycerol residues, in which an organic solvent is added to glycerol residues, followed by heating and stirring, followed by two-stage extraction, decolorization, and two-stage filtration, to obtain a polyglycerol product. However, in the preparation method, a large amount of organic solvent (1 to 20 times of organic solvent such as alcohol, acetone, ether and the like) is required to be added for extraction, potential safety hazards exist in the production process, the production cost is high, the content purity of the polyglycerol obtained by secondary molecular distillation is not high, only 80 percent is reached, and the requirements of food grade and cosmetic grade are not met.
Disclosure of Invention
In order to solve the defects and shortcomings of the prior art, the invention aims to provide the method for extracting the polyglycerol from the glycerol slag, which solves the problem of molecular distillation of monoglyceride leftovers (glycerol slag) for many years, saves certain production cost for companies, saves energy, reduces consumption, and is safe and environment-friendly.
The invention is realized by the following technical scheme:
a method for extracting polyglycerol from glycerol slag comprises the following steps of treating the glycerol slag and performing molecular rectification on a glycerol primary product:
(1) preparing a glycerol residue solution: according to the mass ratio of 1: (0.5-6) weighing the glycerin residue and water, uniformly mixing the glycerin residue and the water, and heating to boil until the glycerin residue and the water are dissolved into liquid to obtain a glycerin residue solution;
(2) preparation of the separating agent solution: weighing a separating agent and water according to a mass ratio of 1 (200-600), and dissolving the separating agent in the water to form a colloidal water sample to obtain a separating agent solution;
(3) demulsification and separation: slowly adding the separating agent solution in the step (2) into the glycerol residue solution in the step (1), heating and stirring, cooling, standing and separating into a supernatant and a lower emulsion, filtering to obtain the supernatant which is a glycerol primary product, and the lower emulsion which is an ester and phosphate solid mixture;
(4) molecular rectification of a glycerol primary product: and (4) treating the primary glycerol product obtained in the step (3) by a three-stage molecular distillation process to remove impurities such as free glycerol, ester compounds and the like, wherein the obtained distillation product is polyglycerol.
Preferably, the heating temperature in the step (1) is 80-100 ℃.
Preferably, the heating temperature in the step (1) is 95 ℃.
Preferably, the separating agent in the step (2) is at least one of a flocculating agent and a demulsifying agent.
Preferably, the standing separation temperature in the step (3) is 80-100 ℃, and the standing heat preservation time is 1-30 minutes; the filtration is carried out by adopting a mode of filter cloth or a filter frame or a filter screen or filter paper; the solids obtained by filtering the lower emulsion were a mixture of ester and phosphate solids.
Preferably, the vacuum pressure of the first-stage molecular distillation in the step (4) is 200-2000 Pa, and the temperature is 80-180 ℃, so as to remove air and moisture; the vacuum pressure of the second-stage molecular distillation is 150-1000 Pa, and the temperature is 120-200 ℃, so that the purpose is to separate free glycerin; the vacuum pressure of the third-stage molecular distillation is 10-500 Pa, the temperature is 160-220 ℃, and the aim is to continuously separate the free glycerin to obtain the high-purity polyglycerol with the purity of more than 95%.
In a preferable scheme, the vacuum pressure of the first-stage molecular distillation is 200Pa, and the temperature is 100 ℃; the vacuum pressure of the second-stage molecular distillation is 100Pa, and the temperature is 160 ℃; the vacuum pressure of the third-stage molecular distillation is 10Pa, and the temperature is 200 ℃.
Preferably, the vacuum pressure of the first-stage molecular distillation is 1000Pa, and the temperature is 110 ℃; the vacuum pressure of the second-stage molecular distillation is 200Pa, and the temperature is 180 ℃; the vacuum pressure of the third-stage molecular distillation is 10Pa, and the temperature is 200 ℃.
In a preferred further scheme, the vacuum pressure of the first-stage molecular distillation is 1500Pa, and the temperature is 130 ℃; the vacuum pressure of the second-stage molecular distillation is 150Pa, and the temperature is 190 ℃; the vacuum pressure of the third-stage molecular distillation is 20Pa, and the temperature is 210 ℃.
As still another preferred embodiment, the first molecular distillation stage has a vacuum pressure of 2000Pa and a temperature of 130 ℃; the vacuum pressure of the second-stage molecular distillation is 300Pa, and the temperature is 200 ℃; the vacuum pressure of the third-stage molecular distillation is 10Pa, and the temperature is 208 ℃.
The glycerin residue includes but is not limited to the following parts: one or more of saturated or unsaturated, fully hydrogenated or partially hydrogenated and even non-hydrogenated raw oil of industries such as molecular distillation glycerin monostearate, molecular distillation monopalmitin, molecular distillation glycerin monolaurate, molecular distillation glycerin monooctyl decanoate, molecular distillation glycerin citrate and the like.
The principle of the invention is as follows:
mixing a prepared glycerol slag solution and a separating agent solution, heating and stirring, cooling and standing to separate into a supernatant and a lower emulsion, filtering to obtain the supernatant which is a glycerol primary product, and the lower emulsion is an ester and phosphate solid mixture; then the obtained glycerin primary product is treated by a three-stage molecular distillation process to remove impurities such as free glycerin, ester compounds and the like, and the obtained distillation product is polyglycerol; the molecular distillation is a distillation method operated under high vacuum, is a special liquid-liquid separation technology, and is different from the traditional distillation and relies on the boiling point difference separation principle, but relies on the difference of different substance molecular motion mean free path to realize the separation.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the method for preparing the polyglycerol from the leftovers (waste glycerol residues) has high purity and the content of the polyglycerol reaches more than 95 percent. Is a method for extracting, separating, distilling and purifying polyglycerol from the bottom glycerol slag of molecular distillation monoglyceride; the method solves the problem of solid waste discharge of the glycerol slag of the current molecular distillation monoglyceride manufacturers, has the advantages of changing waste into valuables with the maximum efficiency, saving energy, reducing consumption and being capable of being directly used for food-grade and cosmetic-grade raw materials, solves the problem of industrial circulation of the molecular distillation industry, saves energy and protects the environment, and the product prepared by the method has good quality and light color, and the content of polyglycerol in the product reaches more than 95 percent.
(2) The process adopts molecular distillation, the temperature in the distillation process is low, and the separation purpose can be achieved as long as the temperature difference exists; the distillation vacuum degree is high, so that the material is not easy to oxidize and damage; the distilled liquid film is thin, the heat transfer efficiency is high, the energy consumption of the product is low, the heat loss in the whole separation process of molecular distillation is low, the internal pressure is extremely low, and the energy consumption can be greatly saved; the heating time of the material is short, the retention time at the distillation temperature is generally between a few seconds and dozens of seconds, and the chance of thermal decomposition of the material is reduced; the separation degree is higher, and the molecular distillation can separate substances which are not easy to separate conventionally; the molecular distillation has no boiling bubbling phenomenon, the molecular distillation is free evaporation on the surface of a liquid layer and is carried out under low pressure, and no dissolved air exists in the liquid, so that the whole liquid can not be boiled in the distillation process and no bubbling phenomenon exists; the whole production process is non-toxic, harmless, pollution-free and residue-free, and a pure and safe product can be obtained; can selectively evaporate the target product, remove other impurities, and can simultaneously separate more than 2 substances through multi-stage separation; the fractionation process of molecular distillation is a physical process and thus provides good protection against contamination and attack of the separated material.
(3) The process adopts three-stage molecular distillation, has the advantages of separating the polyglycerol from the waste glycerol slag by adding water and a separating agent, and has high purity, compared with the traditional two-stage molecular distillation, the process adopts the steps of adding 0.5 to 6 times of water and a small amount of separating agent, demulsifying and separating ester substances and phosphate to obtain a crude glycerol aqueous solution, decoloring, and dehydrating and removing the glycerol by the three-stage molecular distillation to obtain the polyglycerol. Generally, a large amount of 1 to 20 times of organic solvent (such as alcohol, acetone, ether and the like) is added conventionally, phosphate is separated through extraction (potential safety and environmental protection hazards exist in the production process), and the content of polyglycerol is about 80% after decolorization and secondary molecular distillation. The polyglycerol obtained by three-stage molecular distillation contains more than 95% of ester compounds, has a free glycerol content of 0.1-0.6%, is a light yellow viscous liquid, and can be esterified with hydrogenated oil or hardened oil to prepare polyglycerol ester.
Drawings
FIG. 1 is a flow chart of a glycerin residue treatment process;
FIG. 2 is a schematic diagram of a process flow of molecular distillation of a primary glycerol product.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
The method for extracting polyglycerol from glycerol slag comprises the following steps of treating the glycerol slag and rectifying a primary glycerol product:
(1) preparing a glycerol residue solution: according to the mass ratio of 1: (0.5-6) weighing the glycerin residue and water, uniformly mixing the glycerin residue and the water, and heating to boil until the glycerin residue and the water are dissolved into liquid to obtain a glycerin residue solution;
(2) preparation of the separating agent solution: weighing a separating agent and water according to a mass ratio of 1 (200-600), and dissolving the separating agent in the water to form a colloidal water sample to obtain a separating agent solution;
(3) demulsification and separation: slowly adding the separating agent solution in the step (2) into the glycerol residue solution in the step (1), heating and stirring to 95 ℃, keeping the temperature for 1 to 30 minutes until the upper glycerol solution is transparent, standing and separating, then filtering to obtain the upper clear liquid which is a glycerol primary product and the lower emulsion which is a solid mixture of ester and phosphate;
the upper layer is a glycerin primary product accounting for about 80% of the total amount, and the lower layer is a mixture of esters and phosphate accounting for about 20% of the total amount, and is sold as animal feed.
(4) Molecular rectification of a glycerol primary product: and (4) treating the glycerin primary product obtained in the step (3) by a three-stage molecular distillation process to remove free glycerin, ester compounds and other impurities, and obtaining a distilled product, namely the polyglycerol.
The glycerin residue includes but is not limited to the following parts: one or more of saturated or unsaturated, fully hydrogenated or partially hydrogenated and even non-hydrogenated raw oil of industries such as molecular distillation glycerin monostearate, molecular distillation monopalmitin, molecular distillation glycerin monolaurate, molecular distillation glycerin monooctyl decanoate, molecular distillation glycerin citrate and the like. Wherein the raw materials for producing molecular distillation glycerin monostearate, molecular distillation glycerin monopalmitate, molecular distillation glycerin monolaurate, molecular distillation glycerin monooctate and molecular distillation glycerin citrate can be natural animal and vegetable oils and interesterified, modified oils, such as: soybean oil, palm kernel oil, lard, beef tallow, mutton fat, peanut oil, sunflower oil, safflower oil, deep sea fish oil, cocoa butter, cotton seed oil, sardine oil, sea buckthorn oil and other fully or partially hydrogenated oils or mixtures of several oils.
Example 1
Taking 500 g of glycerin residue after the production of the molecular distillation ester emulsifier and simultaneously taking 1000 g of water, uniformly mixing the glycerin residue and the water, and heating to boil until the glycerin residue is dissolved into liquid to obtain a glycerin residue solution; then 0.25 g of separating agent and 100 g of water are respectively weighed and the separating agent is put into the water to be dissolved into a colloidal water sample to obtain a separating agent solution; slowly adding the separating agent solution into the glycerol residue solution, heating, stirring, cooling, standing, and separating into upper clear liquid and lower emulsion, wherein the upper clear liquid is glycerol primary product, and the lower emulsion is solid mixture of ester and phosphate (the lower substance is sold as pig feed and animal feed); filtering the supernatant with a filter frame to obtain a filtrate as a glycerol primary product, wherein the specific flow is shown in figure 1.
Introducing the primary glycerol product into a three-stage molecular distillation system, and keeping the vacuum pressure of the primary molecular distillation at 1000Pa and the temperature at 110 ℃ for removing air and moisture; the vacuum pressure of the second molecular distillation is 200Pa and the temperature is 180 ℃ in order to separate the free glycerol; the vacuum pressure of the third molecular distillation was 10Pa, the temperature was 200 ℃ for the purpose of continuing to separate the free glycerol to obtain high purity polyglycerol, and 356.2 g of polyglycerol was obtained by distillation, as shown in FIG. 2. The mass fraction content of the polyglycerol detected by the gas chromatography of Agilent 7820 in America is 97.1 percent and is in accordance with the standard GB 1886.65-2015.
Example 2
Taking 500 g of glycerin residue after the production of the molecular distillation ester emulsifier and simultaneously taking 1000 g of water, uniformly mixing the glycerin residue and the water, and heating to boil until the glycerin residue is dissolved into liquid to obtain a glycerin residue solution; then 0.25 g of separating agent and 100 g of water are respectively weighed and the separating agent is put into the water to be dissolved into a colloidal water sample to obtain a separating agent solution; slowly adding the separating agent solution into the glycerol residue solution, heating, stirring, cooling, standing, and separating into upper clear liquid and lower emulsion, wherein the upper clear liquid is glycerol primary product, and the lower emulsion is solid mixture of ester and phosphate (the lower substance is sold as pig feed and animal feed); filtering the supernatant with a filter frame to obtain a filtrate as a glycerol primary product, wherein the specific flow is shown in figure 1.
Introducing the glycerol primary product into a three-stage molecular distillation system, and keeping the vacuum pressure of the first-stage molecular distillation at 1500Pa and the temperature at 130 ℃ for removing air and moisture; the vacuum pressure of the second molecular distillation was 150Pa and the temperature was 190 ℃ in order to separate the free glycerol; the vacuum pressure of the third molecular distillation was 20Pa and the temperature was 210 ℃ in order to continue separating the free glycerol to obtain high purity polyglycerol, which was distilled to obtain 366.2 g of polyglycerol, as shown in FIG. 1. The mass fraction content of the polyglycerol detected by the gas chromatography of Agilent 7820 in America is 95.9 percent and is in accordance with the standard GB 1886.65-2015.
Example 3
Taking 500 g of glycerin residue after the production of the molecular distillation ester emulsifier and simultaneously taking 1000 g of water, uniformly mixing the glycerin residue and the water, and heating to boil until the glycerin residue is dissolved into liquid to obtain a glycerin residue solution; then 0.25 g of separating agent and 100 g of water are respectively weighed and the separating agent is put into the water to be dissolved into a colloidal water sample to obtain a separating agent solution; slowly adding the separating agent solution into the glycerol residue solution, heating, stirring, cooling, standing, and separating into upper clear liquid and lower emulsion, wherein the upper clear liquid is the primary polyglycerol product, and the lower emulsion is the solid mixture of ester and phosphate (the lower substance is sold as pig feed and animal feed); filtering the supernatant with a filter frame to obtain a filtrate as a glycerol primary product, wherein the specific flow is shown in figure 1.
Putting the initial product of polyglycerol into a three-stage molecular distillation system, and keeping the vacuum pressure of the first-stage molecular distillation at 200Pa and the temperature at 100 ℃ for removing air and moisture; the vacuum pressure of the second molecular distillation is 100Pa and the temperature is 160 ℃, in order to separate the free glycerol; the vacuum pressure of the third molecular distillation was 10Pa, the temperature was 200 ℃ for the purpose of continuing to separate the free glycerol to obtain high purity polyglycerol, which was distilled to obtain 358.8 g of polyglycerol, as shown in FIG. 2. Adopts an Agilent 7820 gas chromatography in America to detect that the content of the mass fraction of the polyglycerol is 99.1 percent according to the standard GB 1886.65-2015.
Example 4
Taking 500 g of glycerin residue after the production of the molecular distillation ester emulsifier and simultaneously taking 1000 g of water, uniformly mixing the glycerin residue and the water, and heating to boil until the glycerin residue is dissolved into liquid to obtain a glycerin residue solution; then 0.25 g of separating agent and 100 g of water are respectively weighed and the separating agent is put into the water to be dissolved into a colloidal water sample to obtain a separating agent solution; slowly adding the separating agent solution into the glycerol residue solution, heating, stirring, cooling, standing, and separating into upper clear liquid and lower emulsion, wherein the upper clear liquid is glycerol primary product, and the lower emulsion is solid mixture of ester and phosphate (the lower substance is sold as pig feed and animal feed); filtering the supernatant with a filter frame to obtain a filtrate as a glycerol primary product, wherein the specific flow is shown in figure 1.
Introducing the glycerol primary product into a three-stage molecular distillation system, and keeping the vacuum pressure of the first-stage molecular distillation at 2000Pa and the temperature at 130 ℃ for removing air and moisture; the vacuum pressure of the second molecular distillation is 300Pa and the temperature is 200 ℃, in order to separate the free glycerol; the vacuum pressure of the third molecular distillation was 10Pa, the temperature was 208 deg.C, the purpose was to continue to separate the free glycerol to obtain high purity polyglycerol, and 356.2 g of polyglycerol was obtained by distillation, the specific procedure is shown in FIG. 2. The mass fraction content of the polyglycerol detected by the gas chromatography of Agilent 7820 in America is 96.8%, and the detection standard is in accordance with GB 1886.65-2015.
Example 5
Taking 600 g of glycerin residue after the production of the molecular distillation ester emulsifier, simultaneously taking 1500 g of water, uniformly mixing the glycerin residue and the water, heating to boiling until the glycerin residue is dissolved into liquid, and obtaining a glycerin residue solution; then 0.30 g of separating agent and 120 g of water are respectively weighed and the separating agent is put into the water to be dissolved into a colloidal water sample to obtain a separating agent solution; slowly adding the separating agent solution into the glycerol residue solution, heating, stirring, cooling, standing, and separating into upper clear liquid and lower emulsion, wherein the upper clear liquid is the primary polyglycerol product, and the lower emulsion is the solid mixture of ester and phosphate (the lower substance is sold as pig feed and animal feed); filtering the supernatant with a filter frame to obtain a filtrate as a glycerol primary product, wherein the specific flow is shown in figure 1.
Putting the initial product of polyglycerol into a three-stage molecular distillation system, and keeping the vacuum pressure of the first-stage molecular distillation at 200Pa and the temperature at 100 ℃ for removing air and moisture; the vacuum pressure of the second molecular distillation is 100Pa and the temperature is 160 ℃, in order to separate the free glycerol; the vacuum pressure of the third stage molecular distillation is 10Pa, the temperature is 200 ℃, the purpose is to continuously separate the free glycerin to obtain the high-purity polyglycerin, and the specific flow chart is shown in figure 2. The mass fraction content of the polyglycerol detected by the gas chromatography of Agilent 7820 in America is 96.8%, and the detection standard is in accordance with GB 1886.65-2015.
Example 6
Taking 1000 g of glycerin residue after the production of the molecular distillation ester emulsifier and 3000 g of water at the same time, uniformly mixing the glycerin residue and the water, heating to boiling until the glycerin residue is dissolved into liquid, and obtaining a glycerin residue solution; then 0.66 g of separating agent and 200 g of water are respectively weighed and the separating agent is put into the water to be dissolved into a colloidal water sample to obtain a separating agent solution; slowly adding the separating agent solution into the glycerol residue solution, heating, stirring, cooling, standing, and separating into upper clear liquid and lower emulsion, wherein the upper clear liquid is the primary polyglycerol product, and the lower emulsion is the solid mixture of ester and phosphate (the lower substance is sold as pig feed and animal feed); filtering the supernatant with a filter frame to obtain a filtrate as a glycerol primary product, wherein the specific flow is shown in figure 1.
Putting the initial product of polyglycerol into a three-stage molecular distillation system, and keeping the vacuum pressure of the first-stage molecular distillation at 200Pa and the temperature at 100 ℃ for removing air and moisture; the vacuum pressure of the second molecular distillation is 100Pa and the temperature is 160 ℃, in order to separate the free glycerol; the vacuum pressure of the third stage molecular distillation is 10Pa, the temperature is 200 ℃, the aim is to continuously separate the free glycerol to obtain the high-purity polyglycerol, and the specific flow chart is as shown in figure 2. The content of the polymerized glycerol in mass fraction is 97.2 percent through gas phase detection, and the detection standard is in accordance with GB 1886.65-2015.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A method for extracting polyglycerol from glycerol slag is characterized by comprising the following steps of treating the glycerol slag and rectifying a primary glycerol product:
(1) preparing a glycerol residue solution: according to the mass ratio of 1: (0.5-6) weighing the glycerin residue and water, uniformly mixing the glycerin residue and the water, and heating to boil until the glycerin residue and the water are dissolved into liquid to obtain a glycerin residue solution;
(2) preparation of the separating agent solution: weighing a separating agent and water according to a mass ratio of 1 (200-600), and dissolving the separating agent in the water to form a colloidal water sample to obtain a separating agent solution;
(3) demulsification and separation: slowly adding the separating agent solution in the step (2) into the glycerol residue solution in the step (1), heating and stirring, cooling, standing and separating into a supernatant and a lower emulsion, filtering to obtain the supernatant which is a glycerol primary product, and the lower emulsion which is an ester and phosphate solid mixture;
(4) molecular rectification of a glycerol primary product: and (4) treating the primary glycerol product obtained in the step (3) by a three-stage molecular distillation process to remove impurities such as free glycerol, ester compounds and the like, wherein the obtained distillation product is polyglycerol.
2. The method for extracting polyglycerol from glycerol slag according to claim 1, wherein: the heating temperature in the step (1) is 80-100 ℃.
3. The method for extracting polyglycerol from glycerol slag according to claim 1, wherein: the separating agent in the step (2) is at least one of a flocculating agent and a demulsifier.
4. The method for extracting polyglycerol from glycerol slag according to claim 1, wherein: the standing separation temperature in the step (3) is 80-100 ℃, and the standing heat preservation time is 1-30 minutes; the filtration is carried out by adopting a mode of filter cloth or a filter frame or a filter screen or filter paper; the solids obtained by filtering the lower emulsion were a mixture of ester and phosphate solids.
5. The method for extracting polyglycerol from glycerol slag according to claim 1, wherein: the vacuum pressure of the first-stage molecular distillation in the step (4) is 200-2000 Pa, and the temperature is 80-180 ℃; the vacuum pressure of the second-stage molecular distillation is 150-1000 Pa, and the temperature is 120-200 ℃; the vacuum pressure of the third-stage molecular distillation is 10-500 Pa, and the temperature is 160-220 ℃.
6. The method for extracting polyglycerol from glycerol slag according to claim 5,
the vacuum pressure of the first-stage molecular distillation is 200Pa, and the temperature is 100 ℃; the vacuum pressure of the second-stage molecular distillation is 100Pa, and the temperature is 160 ℃; the vacuum pressure of the third-stage molecular distillation is 10Pa, and the temperature is 200 ℃.
7. The method for extracting polyglycerol from glycerol residues according to claim 5, wherein the vacuum pressure of the first stage molecular distillation is 1000Pa, and the temperature is 110 ℃; the vacuum pressure of the second-stage molecular distillation is 200Pa, and the temperature is 180 ℃; the vacuum pressure of the third-stage molecular distillation is 10Pa, and the temperature is 200 ℃.
8. The method for extracting polyglycerol from glycerol residues according to claim 5, wherein the vacuum pressure of the first stage molecular distillation is 1500Pa, and the temperature is 130 ℃; the vacuum pressure of the second-stage molecular distillation is 150Pa, and the temperature is 190 ℃; the vacuum pressure of the third-stage molecular distillation is 20Pa, and the temperature is 210 ℃.
9. The method for extracting polyglycerol from glycerol residues according to claim 5, wherein the vacuum pressure of the first stage molecular distillation is 2000Pa, and the temperature is 130 ℃; the vacuum pressure of the second-stage molecular distillation is 300Pa, and the temperature is 200 ℃; the vacuum pressure of the third-stage molecular distillation is 10Pa, and the temperature is 208 ℃.
10. The method for extracting polyglycerol from glycerol slag according to any one of claims 1 to 9, wherein the glycerol slag comprises but is not limited to the following: one or more of saturated or unsaturated, fully hydrogenated or partially hydrogenated and even non-hydrogenated raw oil of industries such as molecular distillation glycerin monostearate, molecular distillation monopalmitin, molecular distillation glycerin monolaurate, molecular distillation glycerin monooctyl decanoate, molecular distillation glycerin citrate and the like.
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| CN115247097A (en) * | 2022-07-27 | 2022-10-28 | 四川天宇油脂化学有限公司 | Concrete release agent based on glycerol extract and preparation method thereof |
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Application publication date: 20200124 |