CN110918064A - Environment-friendly industrial waste glycerol recovery process - Google Patents
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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Abstract
The invention discloses an environment-friendly industrial waste glycerol recovery process, which comprises the following steps: step one, modification of diatomite: firstly, pre-activating the diatomite, then adding the diatomite into a magnetic stirrer, then adding a chitosan solution 2 times of the total amount of the diatomite, stirring the mixture at the rotating speed of 200-300r/min for 30-40min, and finishing stirring. The diatomite is pretreated, the surface activity can be obviously improved, the subsequent treatment of a chitosan solution is convenient, the chitosan solution is formed by compounding phosphoric acid and chitosan, the capability of chitosan entering the diatomite through a microporous structure of the diatomite is improved, the capability of the diatomite for adsorbing glycerol is enhanced after the chitosan is used for treating the diatomite, and finally the modified rice hull ash is compounded, so that the surface porosity of the modified rice hull ash is improved after the modification treatment, the specific surface area is large, and the adsorption effect is improved after the modified rice hull ash is compounded with the diatomite.
Description
Technical Field
The invention relates to the technical field of glycerol recovery, in particular to an environment-friendly industrial waste glycerol recovery process.
Background
Glycerol is a colorless, sweet, clear, viscous liquid, odorless, warm and sweet, and can absorb moisture from the air, hydrogen sulfide, hydrogen cyanide, and sulfur dioxide. Insoluble in benzene, chloroform, carbon tetrachloride, carbon disulfide, petroleum ether and oils. Relative density 1.26362. Melting point 17.8 ℃. Boiling point 290.0 deg.C, refractive index 1.4746. The boiling point of glycerin is as high as 290 ℃, so that the glycerin can be used for preparing various resins in the paint industry, but the glycerin is easy to yellow at high temperature, thereby affecting the product quality of the paint.
Most of the existing industrial glycerin is discarded after being used, so that not only is resources wasted, but also certain damage is caused to the environment, and the existing environmental protection concept is not met.
The prior Chinese patent document No. CN106588566B discloses a glycerol recovery process, which comprises the following processing steps: firstly, setting a drying room, putting crude oil into the drying room for melting, wherein the temperature in the drying room is 70-120 ℃, and a molten pool for storing the melted crude oil is arranged in the drying room; conveying the crude oil in the molten pool to a hydrolysis kettle, controlling the temperature of the hydrolysis kettle at 220-280 ℃, and performing hydrolysis reaction on the crude oil and water vapor under the conditions of high temperature and normal pressure to obtain fatty acid, water vapor, crude glycerol and grease through hydrolysis; and thirdly, the liquid hydrolyzed in the second step is cooled by water, the crude glycerol is settled at the bottom through static layer separation, the crude glycerol is sent to a separator for the first gasoline separation, the temperature in the separator is controlled at 180 ℃, water vapor is evaporated, the water vapor flows back to the hydrolysis kettle for use, and the crude glycerol is sent to a storage tank.
Disclosure of Invention
The invention aims to provide an environment-friendly industrial waste glycerol recovery process to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides an environment-friendly industrial waste glycerol recovery process, which comprises the following steps:
step one, modification of diatomite: firstly, pre-activating diatomite, then adding the diatomite into a magnetic stirrer, then adding a chitosan solution 2 times of the total amount of the diatomite, stirring the mixture at the rotating speed of 200-300r/min for 30-40min, and finishing stirring;
step two, preparing the composite adsorbent: feeding the modified diatomite obtained in the step one and the modified rice hull ash accounting for 20-50% of the total weight of the diatomite into a high-pressure reaction kettle containing an ethanol solvent, stirring for 5-9h at the high pressure of 10-20MPa and the rotating speed of 300-400r/min, and obtaining the composite adsorbent after the reaction is finished;
step three, preparing a flexible rebound agent: adding silicon dioxide microspheres into triglyceride, sequentially adding sodium hyaluronate and camellia seed oil, stirring for 1-2h at 55-65 ℃ at a rotating speed of 400r/min at 300-;
step four, pretreatment of the composite adsorbent: the composite adsorbent is firstly sent into sodium citrate for treatment for 15-25min, then centrifugation and drying are carried out, then the epoxidized soybean oil after ring opening is added into the composite adsorbent treated by the sodium citrate, and then the mixture is stirred for 50-60min at the rotating speed of 100 r/min;
step five, preparation of a recycling agent: sending the composite adsorbent pretreated in the fourth step into the flexible resilient agent prepared in the third step, performing ultrasonic dispersion for 10-20min at the ultrasonic power of 100-200W, then stirring for 5-9h at the low rotating speed of 100-150r/min at 75 ℃, after stirring, washing, centrifuging and drying to obtain a recycling agent;
and step six, adding the recycling agent obtained in the step five into the waste glycerin, stirring, taking out the recycling agent after stirring is finished, and recycling the waste glycerin under the condition of 5-15 MPa.
The invention further comprises the following steps: the pre-activation treatment comprises the specific steps of firstly carrying out primary activation treatment on the diatomite under the condition of inert gas, calcining the diatomite for 1.5-2.5h at the temperature of 250-290 ℃, then cooling the diatomite to the room temperature at the speed of 2-5 ℃/min, and then carrying out secondary activation treatment.
The invention further comprises the following steps: the secondary activation treatment is that the diatomite is sent into a plasma reaction cavity, then nitrogen and argon are sequentially introduced into the plasma reaction cavity, the nitrogen is introduced for 15-25min, the argon is introduced for 5-10min, and the gas flow is 1.5-2.5L/min.
The invention further comprises the following steps: in the first step, chitosan solution with pH of 5.5-5.9 is prepared from chitosan and phosphoric acid according to the weight ratio of 1: 2.
The invention further comprises the following steps: the preparation method of the modified rice hull ash comprises the step of adding the rice hull ash into FeCl3Ultrasonic dispersion is carried out in the solution for 10-20min with the ultrasonic power of 100-200W, then centrifugation and drying are carried out, and ZnCl is adopted3And performing secondary ultrasonic dispersion on the solution, and finally centrifuging, washing and drying to obtain the modified rice hull ash.
The invention further comprises the following steps: the secondary ultrasonic dispersion time is 20-30min, and the ultrasonic power is 150-250W.
The invention further comprises the following steps: the secondary ultrasonic dispersion time is 25min, and the ultrasonic power is 200W.
The invention further comprises the following steps: the preparation condition of the ring-opened epoxy soybean oil is ring opening under the condition of sodium methoxide alkaline catalyst, the ring opening temperature is 115-125 ℃, and the reaction lasts for 3-6 h.
The invention further comprises the following steps: the ring opening temperature is 120 ℃, and the reaction lasts for 4.5 h.
Compared with the prior art, the invention has the following beneficial effects:
(1) the diatomite is pretreated, the surface activity can be obviously improved, the subsequent treatment of a chitosan solution is convenient, the chitosan solution is formed by compounding phosphoric acid and chitosan, the capability of chitosan entering the diatomite through a microporous structure of the diatomite is improved, the capability of the diatomite for adsorbing glycerol is enhanced after the chitosan is used for treating the diatomite, and finally the modified rice hull ash is compounded, so that the surface porosity of the modified rice hull ash is improved after the modification treatment, the specific surface area is large, and the adsorption effect is improved after the modified rice hull ash is compounded with the diatomite.
(2) The composite adsorbent is treated by sodium citrate firstly, then treated by epoxidized soybean oil after ring opening, the epoxidized soybean oil after ring opening is coated on the surface of the composite adsorbent, so that the contact effect with the waste glycerol is improved, the glycerol can be removed after the recovery agent after absorbing the glycerol is treated under high pressure, and meanwhile, the original structure can be recovered after being treated by the flexible rebound agent, so that the composite adsorbent can be recycled, the waste glycerol is absorbed again, and the utilization effect is improved.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the environment-friendly industrial waste glycerol recovery process comprises the following steps:
step one, modification of diatomite: firstly, pre-activating diatomite, then adding the diatomite into a magnetic stirrer, then adding a chitosan solution 2 times of the total amount of the diatomite, stirring at the rotating speed of 200r/min for 30min, and finishing stirring;
step two, preparing the composite adsorbent: feeding the modified diatomite obtained in the step one and the modified rice hull ash accounting for 20% of the total amount of the diatomite into a high-pressure reaction kettle containing an ethanol solvent, stirring for 5 hours at the high pressure of 10MPa and at the rotating speed of 300r/min, and obtaining a composite adsorbent after the reaction is finished;
step three, preparing a flexible rebound agent: adding silicon dioxide microspheres into triglyceride, sequentially adding sodium hyaluronate and camellia seed oil, stirring at 55 ℃ for 1h at a rotating speed of 300r/min in a reaction kettle, adding sorbitol solution, continuously stirring for 20min, and stirring to obtain a flexible resilient agent;
step four, pretreatment of the composite adsorbent: the composite adsorbent is firstly sent into sodium citrate for treatment for 15min, then is centrifuged and dried, and then the epoxidized soybean oil after ring opening is added into the composite adsorbent treated by the sodium citrate, and then is stirred for 50min at the rotating speed of 100 r/min;
step five, preparation of a recycling agent: sending the composite adsorbent pretreated in the fourth step into the flexible rebound agent prepared in the third step, performing ultrasonic dispersion for 10min at 100W ultrasonic power, then stirring for 5h at 75 ℃ and low rotation speed of 100r/min, after stirring, washing, centrifuging and drying to obtain a recovery agent;
and step six, adding the recycling agent obtained in the step five into the waste glycerin, stirring, taking out the recycling agent after stirring is finished, and recycling the waste glycerin under the condition of 5 MPa.
The specific steps of the pre-activation treatment in this example are to perform a first activation treatment on the diatomite under an inert gas condition, calcine the diatomite at 250 ℃ for 1.5h in the first activation treatment, then reduce the temperature to room temperature at a rate of 2 ℃/min, and then perform a second activation treatment.
In the second activation treatment of this embodiment, diatomite is fed into the plasma reaction chamber, and then nitrogen and argon are sequentially introduced into the plasma reaction chamber, wherein the nitrogen is introduced for 15min, the argon is introduced for 5min, and the gas flow rate is 1.5L/min.
In the first step of this example, a chitosan solution with a pH of 5.5 is prepared from chitosan and phosphoric acid according to a weight ratio of 1: 2.
The modified rice hull ash of this example was prepared by adding rice hull ash to FeCl3Ultrasonic dispersing in the solution for 10min with ultrasonic power of 100W, centrifuging, drying, and then adopting ZnCl3And performing secondary ultrasonic dispersion on the solution, and finally centrifuging, washing and drying to obtain the modified rice hull ash.
The secondary ultrasonic dispersion time of this example was 20min, and the ultrasonic power was 150W.
The preparation conditions of the ring-opened epoxidized soybean oil in the embodiment are ring opening under the condition of sodium methoxide alkaline catalyst, the ring opening temperature is 115 ℃, and the reaction lasts for 3 hours.
Example 2:
the environment-friendly industrial waste glycerol recovery process comprises the following steps:
step one, modification of diatomite: firstly, pre-activating diatomite, then adding the diatomite into a magnetic stirrer, then adding a chitosan solution 2 times of the total amount of the diatomite, stirring at the rotating speed of 300r/min for 40min, and finishing stirring;
step two, preparing the composite adsorbent: feeding the modified diatomite obtained in the step one and the modified rice hull ash accounting for 50% of the total amount of the diatomite into a high-pressure reaction kettle containing an ethanol solvent, stirring for 9 hours at a rotating speed of 400r/min under the high pressure of 20MPa, and finishing the reaction to obtain a composite adsorbent;
step three, preparing a flexible rebound agent: adding silicon dioxide microspheres into triglyceride, sequentially adding sodium hyaluronate and camellia seed oil, stirring in a reaction kettle at 65 ℃ for 2h at a rotating speed of 400r/min, finally adding sorbitol solution, continuously stirring for 30min, and obtaining a flexible resilient agent after stirring;
step four, pretreatment of the composite adsorbent: the composite adsorbent is firstly sent into sodium citrate for treatment for 25min, then is centrifuged and dried, and then the epoxidized soybean oil after ring opening is added into the composite adsorbent treated by the sodium citrate, and then is stirred for 60min at the rotating speed of 100 r/min;
step five, preparation of a recycling agent: sending the composite adsorbent pretreated in the fourth step into the flexible rebound agent prepared in the third step, performing ultrasonic dispersion for 20min at an ultrasonic power of 200W, then stirring for 9h at a low rotation speed of 150r/min at 75 ℃, after stirring, washing, centrifuging and drying to obtain a recovery agent;
and step six, adding the recycling agent obtained in the step five into the waste glycerin, stirring, taking out the recycling agent after stirring is finished, and recycling the waste glycerin under the condition of 15 MPa.
The pre-activation treatment of this example includes the steps of subjecting diatomaceous earth to primary activation treatment under inert gas conditions, calcining diatomaceous earth at 290 ℃ for 2.5 hours, cooling diatomaceous earth to room temperature at a rate of 5 ℃/min, and then subjecting diatomaceous earth to secondary activation treatment.
In the second activation treatment of this embodiment, diatomite is fed into the plasma reaction chamber, and then nitrogen and argon are sequentially introduced into the plasma reaction chamber, wherein the nitrogen is introduced for 25min, the argon is introduced for 10min, and the gas flow rate is 2.5L/min.
In the first step of this example, a chitosan solution with a pH of 5.9 is prepared from chitosan and phosphoric acid according to a weight ratio of 1: 2.
The modified rice hull ash of this example was prepared by adding rice hull ash to FeCl3Ultrasonic dispersing in the solution for 20min with ultrasonic power of 200W, centrifuging, drying, and then adopting ZnCl3And performing secondary ultrasonic dispersion on the solution, and finally centrifuging, washing and drying to obtain the modified rice hull ash.
The secondary ultrasonic dispersion time of this example was 30min, and the ultrasonic power was 250W.
The preparation conditions of the ring-opened epoxidized soybean oil in the embodiment are ring opening under the condition of sodium methoxide alkaline catalyst, the ring opening temperature is 125 ℃, and the reaction is carried out for 6 hours.
Example 3:
the environment-friendly industrial waste glycerol recovery process comprises the following steps:
step one, modification of diatomite: firstly, pre-activating diatomite, then adding the diatomite into a magnetic stirrer, then adding a chitosan solution 2 times of the total amount of the diatomite, stirring at the rotating speed of 250r/min for 35min, and finishing stirring;
step two, preparing the composite adsorbent: feeding the diatomite modified in the step one and the modified rice hull ash accounting for 25% of the total weight of the diatomite into a high-pressure reaction kettle containing an ethanol solvent, stirring for 7 hours at the rotating speed of 350r/min under the high pressure of 15MPa, and finishing the reaction to obtain a composite adsorbent;
step three, preparing a flexible rebound agent: adding silicon dioxide microspheres into triglyceride, sequentially adding sodium hyaluronate and camellia seed oil, stirring in a reaction kettle at 60 ℃ at a rotating speed of 350r/min for 1.5h, adding sorbitol solution, continuously stirring for 25min, and stirring to obtain a flexible resilient agent;
step four, pretreatment of the composite adsorbent: the composite adsorbent is firstly sent into sodium citrate for processing for 20min, then is centrifuged and dried, and then the epoxidized soybean oil after ring opening is added into the composite adsorbent processed by the sodium citrate, and then is stirred for 55min at the rotating speed of 100 r/min;
step five, preparation of a recycling agent: sending the composite adsorbent pretreated in the fourth step into the flexible rebound agent prepared in the third step, performing ultrasonic dispersion for 15min at the ultrasonic power of 150W, then stirring for 7h at the low rotation speed of 125r/min at the temperature of 75 ℃, after stirring, washing, centrifuging and drying to obtain a recycling agent;
and step six, adding the recycling agent obtained in the step five into the waste glycerin, stirring, taking out the recycling agent after stirring is finished, and recycling the waste glycerin under the condition of 10 MPa.
The specific steps of the pre-activation treatment in this example are to perform a first activation treatment on the diatomite under an inert gas condition, calcine the diatomite at 270 ℃ for 2.0h in the first activation treatment, then reduce the temperature to room temperature at a rate of 3.5 ℃/min, and then perform a second activation treatment.
In the second activation treatment of this embodiment, diatomite is fed into the plasma reaction chamber, and then nitrogen and argon are sequentially introduced into the plasma reaction chamber, wherein the nitrogen is introduced for 20min, the argon is introduced for 7.5min, and the gas flow rate is 2.0L/min.
In the first step of this example, a chitosan solution with a pH of 7.0 is prepared from chitosan and phosphoric acid in a weight ratio of 1: 2.
The modified rice hull ash of this example was prepared by adding rice hull ash to FeCl3Ultrasonically dispersing in the solution for 15min with ultrasonic power of 150W, centrifuging, drying, and then adopting ZnCl3And performing secondary ultrasonic dispersion on the solution, and finally centrifuging, washing and drying to obtain the modified rice hull ash.
The secondary ultrasonic dispersion time of this example was 25min, and the ultrasonic power was 200W.
The preparation conditions of the ring-opened epoxidized soybean oil in the embodiment are ring opening under the condition of sodium methoxide alkaline catalyst, the ring opening temperature is 120 ℃, and the reaction time is 4.5 h.
Comparative example 1:
basically the same materials and preparation process as those in example 3, except that Chinese patent publication No. CN106588566B discloses a raw material and method in example 1 of glycerol recovery process.
Examples 1-3 and comparative example 1 the results of the industrial waste glycerol recovery test are as follows:
compared with the comparative example 1, the glycerol adsorption rate of the invention is obviously improved, and meanwhile, the adsorbent can be reused to adsorb the waste glycerol again, thereby improving the utilization effect.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (9)
1. An environment-friendly industrial waste glycerol recovery process is characterized by comprising the following steps:
step one, modification of diatomite: firstly, pre-activating diatomite, then adding the diatomite into a magnetic stirrer, then adding a chitosan solution 2 times of the total amount of the diatomite, stirring the mixture at the rotating speed of 200-300r/min for 30-40min, and finishing stirring;
step two, preparing the composite adsorbent: feeding the modified diatomite obtained in the step one and the modified rice hull ash accounting for 20-50% of the total weight of the diatomite into a high-pressure reaction kettle containing an ethanol solvent, stirring for 5-9h at the high pressure of 10-20MPa and the rotating speed of 300-400r/min, and obtaining the composite adsorbent after the reaction is finished;
step three, preparing a flexible rebound agent: adding silicon dioxide microspheres into triglyceride, sequentially adding sodium hyaluronate and camellia seed oil, stirring for 1-2h at 55-65 ℃ at a rotating speed of 400r/min at 300-;
step four, pretreatment of the composite adsorbent: the composite adsorbent is firstly sent into sodium citrate for treatment for 15-25min, then centrifugation and drying are carried out, then the epoxidized soybean oil after ring opening is added into the composite adsorbent treated by the sodium citrate, and then the mixture is stirred for 50-60min at the rotating speed of 100 r/min;
step five, preparation of a recycling agent: sending the composite adsorbent pretreated in the fourth step into the flexible resilient agent prepared in the third step, performing ultrasonic dispersion for 10-20min at the ultrasonic power of 100-200W, then stirring for 5-9h at the low rotating speed of 100-150r/min at 75 ℃, after stirring, washing, centrifuging and drying to obtain a recycling agent;
and step six, adding the recycling agent obtained in the step five into the waste glycerin, stirring, taking out the recycling agent after stirring is finished, and recycling the waste glycerin under the condition of 5-15 MPa.
2. The process as claimed in claim 1, wherein the pre-activation treatment comprises a first activation treatment of diatomaceous earth under inert gas conditions, a calcination at 290 ℃ for 1.5-2.5h, a temperature reduction at 2-5 ℃/min to room temperature, and a second activation treatment.
3. The environment-friendly industrial waste glycerol recovery process as claimed in claim 2, wherein the secondary activation treatment is that diatomite is fed into the plasma reaction chamber, then nitrogen and argon are sequentially fed into the plasma reaction chamber, the nitrogen is fed for 15-25min, the argon is fed for 5-10min, and the gas flow is 1.5-2.5L/min.
4. The environment-friendly industrial waste glycerol recovery process as claimed in claim 1, wherein in the first step, the chitosan solution is prepared from chitosan and phosphoric acid according to the weight ratio of 1:2 to obtain the chitosan solution with pH of 5.5-5.9.
5. The environment-friendly industrial waste glycerol recovery process as claimed in claim 1, wherein said modified rice hull ash is prepared by adding rice hull ash to FeCl3Ultrasonic dispersion is carried out in the solution for 10-20min with the ultrasonic power of 100-200W, then centrifugation and drying are carried out, and ZnCl is adopted3And performing secondary ultrasonic dispersion on the solution, and finally centrifuging, washing and drying to obtain the modified rice hull ash.
6. The environment-friendly industrial waste glycerol recovery process as claimed in claim 5, wherein the secondary ultrasonic dispersion time is 20-30min, and the ultrasonic power is 150- & lt 250 & gtW.
7. The environment-friendly industrial waste glycerol recovery process as claimed in claim 6, wherein the secondary ultrasonic dispersion time is 25min, and the ultrasonic power is 200W.
8. The process for recovering the environment-friendly industrial waste glycerol according to claim 1, wherein the ring-opened epoxidized soybean oil is prepared under the conditions of ring opening under the condition of sodium methoxide alkaline catalyst at the ring opening temperature of 115-125 ℃ for reaction for 3-6 h.
9. The environment-friendly industrial waste glycerol recovery process as claimed in claim 8, wherein the ring opening temperature is 120 ℃, and the reaction time is 4.5 h.
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