CN111909793A - Pretreatment method of high-chlorine waste grease - Google Patents
Pretreatment method of high-chlorine waste grease Download PDFInfo
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- CN111909793A CN111909793A CN202010818340.0A CN202010818340A CN111909793A CN 111909793 A CN111909793 A CN 111909793A CN 202010818340 A CN202010818340 A CN 202010818340A CN 111909793 A CN111909793 A CN 111909793A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B13/00—Recovery of fats, fatty oils or fatty acids from waste materials
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/02—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils
- C11C1/04—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils by hydrolysis
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
- C11C1/10—Refining by distillation
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
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Abstract
The invention discloses a pretreatment method of waste oil with high chlorine content, which comprises the following steps: a process: waste animal and vegetable fat → adsorption → hydrolysis → continuous drying or continuous distillation; or the process B: waste animal and vegetable fat → acid treatment → liquid separation → drying → adsorption → hydrolysis → continuous drying or continuous distillation. The fatty acid obtained by the A or B process method not only has low metal and phosphorus contents, but also has low chlorine content, and is an ideal pretreatment method of waste grease with high chlorine content.
Description
Technical Field
The invention belongs to the field of energy and chemical industry, and particularly relates to a pretreatment method of high-chlorine waste grease.
Background
The quantity of waste oil produced in China every year is very large, but the waste oil contains a large amount of metal, chlorine and other impurities and can be used as a raw material of a downstream oil utilization process (including oleic acid extraction, industrial solvent preparation and liquid paraffin preparation) only through pretreatment, the impurities are removed only through physical methods such as water washing, adsorption and deodorization in the traditional waste oil pretreatment, the removal effect is not obvious, the quality of downstream products is affected, and the downstream application of the waste oil is limited.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method for pretreating the high-chlorine waste oil is provided, and the fatty acid obtained by the pretreatment method is low in metal and phosphorus contents and low in chlorine content.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: a pretreatment method of waste oil with high chlorine content comprises the following steps:
a process: waste animal and vegetable fat → adsorption → hydrolysis → continuous drying or continuous distillation;
or
And the process B comprises the following steps: waste animal and vegetable fat → acid treatment → liquid separation → drying → adsorption → hydrolysis → continuous drying or continuous distillation.
Sampling and detecting the waste animal and vegetable oil, and adopting the process A when the chlorine content is more than or equal to 10mg/kg, the total metal content is less than or equal to 100mg/kg, and the phosphorus is less than or equal to 10 mg/kg; sampling and detecting the discarded animal and vegetable oil, and adopting the process B when the chlorine content is more than or equal to 10mg/kg, the total metal content is more than 100mg/kg or the phosphorus content is more than 10 mg/kg.
The waste animal and vegetable oil is one or more of waste cooking oil, swill oil, palmitic acid oil, coconut oil and palm oil.
In the process B, the acid treatment comprises the following steps: adding 50-85 wt.% acid aqueous solution into the waste animal and vegetable oil for acid treatment, controlling the temperature to be 60-80 ℃, and controlling the acid treatment time to be 30-60 min; the acid is phosphoric acid or citric acid; the water solution of the acid accounts for 1 to 15 percent of the mass of the waste animal and vegetable oil.
In the process B, the liquid separation step is carried out under the conditions as follows: standing the materials at the temperature of 60-80 ℃, keeping the temperature of the materials at 60-80 ℃ for oil-water separation, and separating liquid to remove wastewater;
in the process B, the drying step is carried out under the following conditions: and (3) carrying out vacuum drying on the residual oil phase after liquid separation at the drying temperature of 90-105 ℃ and the pressure of 50-100mbar until the water content is less than or equal to 0.5 Wt.%.
In the A, B process, the adsorption step: adding adsorbent at 90-120 deg.C for 10-60min, and filtering after adsorption; the addition amount of the adsorbent accounts for 0.5-4% of the mass of the waste animal and vegetable oil or the waste animal and vegetable oil after acid treatment, liquid separation and drying. The adsorbent is one or a mixture of more of acid clay, activated carbon and silica gel; after adsorption, the mechanical impurities in the product are less than 0.02 Wt%.
In the A, B process, the hydrolysis step: hydrolyzing by adopting a medium-high pressure hydrolysis process, and removing generated glycerol after the hydrolysis is finished; the medium-high pressure hydrolysis process conditions are as follows: the mass ratio of oil to water is 10: 1-1: 1, the reaction pressure is 2.5-5.5 MPa, the reaction temperature is 230-255 ℃, the reaction time is 1-8h, and the hydrolysis rate reaches more than 98%.
In the A, B process, the continuous drying or continuous distillation step: sampling and testing the material obtained by hydrolysis, and continuously drying when the total content of metal and phosphorus is less than 30 mg/kg; when the total content of the metal and phosphorus is more than or equal to 30mg/kg, carrying out continuous distillation; the continuous drying conditions are as follows: vacuum degree of 5-50mbar, retention time of 20-60min, and temperature of 90-110 deg.C; the continuous distillation conditions were: vacuum degree of 5-50mbar, retention time of 20-60min, temperature of 230-.
Has the advantages that: by adopting the process A, after the continuous drying treatment is finished, the phosphorus content of the total metal in the obtained fatty acid is less than or equal to 30mg/kg, the water content is less than or equal to 0.1 percent, the chlorine content is less than or equal to 10mg/kg, and the chlorine removal rate reaches more than 90 percent; after the continuous distillation treatment is finished, the content of total metal phosphorus in the obtained fatty acid is less than or equal to 10mg/kg, the water content is less than or equal to 0.1 percent, the chlorine content is less than or equal to 5mg/kg, and the chlorine removal rate reaches more than 90 percent.
By adopting the process B, most metal ions and phospholipids are removed through acid treatment, a part of metal ions and phospholipids of the waste grease are removed through adsorption, then the chlorine content in the waste grease is reduced through hydrolysis, impurities such as metals and the like are removed through distillation to obtain fatty acid, by adopting the process B, after the continuous drying treatment is finished, the phosphorus content of total metals in the obtained fatty acid is less than or equal to 30mg/kg, the water content is less than or equal to 0.1%, the chlorine content is less than or equal to 10mg/kg, and the chlorine removal rate reaches more than 95%; after the continuous distillation treatment is finished, the content of total metal phosphorus in the obtained fatty acid is less than or equal to 10mg/kg, the water content is less than or equal to 0.1 percent, the chlorine content is less than or equal to 5mg/kg, and the chlorine removal rate reaches more than 95 percent.
The fatty acid prepared by the A or B process method not only has low metal and phosphorus contents, but also has low chlorine content, and is an ideal pretreatment method of waste grease with high chlorine content.
Drawings
FIG. 1 is a process flow diagram of pretreatment A of waste grease with high chlorine content;
FIG. 2 is a process flow chart of pretreatment B of waste grease with high chlorine content.
Detailed Description
The method of the present invention will be further described with reference to the accompanying drawings, but the invention is not limited thereto.
Example 1
Taking a illegal cooking oil sample, detecting, wherein the performance index is shown in table 1, the treatment condition of the process A is met, and the specific treatment process is as follows:
1) weighing about 5000g of illegal cooking oil in a reactor, heating to 105 deg.C, controlling pressure at 100mbar, adding 50g of acid clay, reacting for 30min, and filtering to obtain 4932g of illegal cooking oil for use.
2) Adding the illegal cooking oil obtained in the step 1) into a reaction kettle, adding 4932g of distilled water, heating to 250 ℃, keeping the temperature for 6 hours, keeping the reaction pressure at 5MPa, and separating a water layer and an oil layer by using a separating funnel after the reaction is finished to obtain 4658g of an oil layer.
3) Sampling and testing the material obtained by hydrolysis, wherein the metal content is 13.1mg/kg, the phosphorus content is 0.5mg/kg, the condition that the total content of metal and phosphorus is less than 30mg/kg is met, and drying operation is carried out;
and (3) completely adding the fatty acid obtained in the step 2) into the reaction kettle, controlling the vacuum degree to be 25mbar, heating to 105 ℃, keeping for 30min, and drying to obtain the treated illegal cooking oil, wherein the total amount is 4605g, and the performance index is shown in table 2.
Example 2
Taking a palmitic acid oil sample, detecting, wherein the performance indexes are shown in table 1, the treatment conditions of the A process are met, and the specific treatment process is as follows:
1) weighing about 5000g of illegal cooking oil in a reactor, heating to 105 ℃, controlling the pressure at 100mbar, adding 50g of acid clay, reacting for 30min, and filtering to obtain 4921g of illegal cooking oil for later use.
2) Adding the illegal cooking oil obtained in the step 1) into a reaction kettle, adding 4921g of distilled water, heating to 250 ℃, reacting for 6 hours at 5MPa, and separating a water layer and an oil layer by using a separating funnel after the reaction is finished to obtain 4629g of an oil layer.
3) Sampling and testing the material obtained by hydrolysis, wherein the metal content is 39.7mg/kg, the phosphorus content is 5.8mg/kg, the condition that the total content of metal and phosphorus is more than or equal to 30mg/kg is met, and distilling operation is carried out;
and (3) completely adding the fatty acid obtained in the step 2) into the reaction kettle, controlling the vacuum degree to be 5mbar, heating to 270 ℃, keeping for 30min, and distilling off 4280g of fatty acid, wherein the performance indexes are shown in table 2, and 335g of bottom materials.
Example 3
Taking a illegal cooking oil sample, detecting, wherein the performance index is shown in table 1, the treatment condition of the process B is met, and the specific treatment process is as follows:
1) weighing 5000g of the solution in the reactor, heating to 65 ℃, adding 50g of citric acid aqueous solution with the concentration of 50 wt.% for acid treatment for 30 min.
2) After the acid treatment is finished, controlling the temperature of the materials to be 65 ℃, standing for 2h, separating liquid to remove wastewater, and performing vacuum drying on the residual oil phase; drying at 105 deg.C under 60mbar until water content is less than or equal to 0.5 Wt.% to obtain 4948g illegal cooking oil.
3) Weighing the illegal cooking oil obtained in the step 2) into a reactor, heating to 105 ℃, controlling the pressure at 100mbar, adding 49.5g of acid clay, reacting for 30min, and filtering to obtain 4903g of illegal cooking oil for later use.
4) Adding the drainage oil obtained in the step 3) into the reaction kettle, adding 4903g of distilled water, heating to 250 ℃, reacting for 6 hours at 5MPa, and separating a water layer and an oil layer by using a separating funnel after the reaction is finished to obtain 4608g of an oil layer.
5) Sampling and testing the material obtained by hydrolysis, wherein the metal content is 13.5/mg/kg, the phosphorus content is 1.2mg/kg, the condition that the total content of metal and phosphorus is less than 30mg/kg is met, and drying operation is carried out;
and (3) completely adding the fatty acid obtained in the step (4) into the reaction kettle, controlling the vacuum degree to be 25mbar, heating to 105 ℃, keeping for 30min, and drying to obtain treated illegal cooking oil, wherein the total amount is 4567g, and the performance index is shown in Table 2.
Example 4
Taking a mixture sample of the illegal cooking oil and the palm oil, detecting, wherein the performance indexes are shown in table 1, the treatment conditions of the process B are met, and the specific treatment process comprises the following steps:
1) weighing 5000g of the solution in the reactor, heating to 65 ℃, adding 50g of citric acid aqueous solution with the concentration of 50 wt.% for acid treatment for 30 min.
2) After the acid treatment is finished, controlling the temperature of the materials to be 65 ℃, standing for 2h, separating liquid to remove wastewater, and performing vacuum drying on the residual oil phase; drying at 105 deg.C under 60mbar until water content is less than or equal to 0.5 Wt.% to obtain 4933g of swill-cooked dirty oil.
3) Weighing the illegal cooking oil obtained in the step 2) into a reactor, heating to 105 ℃, controlling the pressure at 100mbar, adding 49.5g of acid clay, reacting for 30min, and filtering to obtain 4909g of illegal cooking oil for later use.
4) And (3) completely adding the illegal cooking oil obtained in the step 3) into the reaction kettle, then adding 4909g of distilled water, heating to 250 ℃, keeping the temperature for 6 hours, and separating a water layer and an oil layer by using a separating funnel after the reaction is finished to obtain 4614g of an oil layer.
5) And (3) sampling and testing the material obtained by hydrolysis, wherein the metal content is 59.2/mg/kg, the phosphorus content is 3.5mg/kg, the condition that the total content of metal and phosphorus is more than or equal to 30mg/kg is met, and distilling operation is carried out.
And (3) completely adding the fatty acid obtained in the step (4) into the reaction kettle, controlling the vacuum degree to be 5mbar, heating to 270 ℃, keeping for 30min, and co-distilling to obtain 4261g of fatty acid, wherein the performance indexes are shown in table 2, and 342g of bottom materials.
Comparative example
The processing mode commonly adopted in the industry is as follows:
1) heating 5000g of illegal cooking oil to 80 +/-2 ℃, adding 250g of primary water for hydration treatment, controlling the temperature to be 80 ℃, and reacting for 30 min.
2) After the hydration treatment in the step 1), keeping the material at 80 ℃, standing for 30-120min, separating a water layer, and then drying in vacuum for 30min at 110 ℃ and under the pressure of 100 mbar.
3) And 2) after drying, heating to 105 ℃, controlling the pressure at 100mbar, adding 50g of acid clay, and reacting for 30 min.
4) And 3) cooling to 80 ℃, separating and filtering argil to obtain 4885g of the impurity-removed illegal cooking oil.
Table 1: the properties of the waste animal and vegetable oil raw materials before treatment in the examples are as follows:
table 2: performance index of fatty acid obtained in examples 1 to 4 and comparative example
| Item | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example |
| Acid value/(mgKOH/g) | 219.6 | 230.1 | 222.6 | 226.2 | 128.3 |
| Metal content/mg/kg | 13.2 | 2.1 | 13.6 | 2.6 | 46.2 |
| Phosphorus content/mg/kg | 1.6 | 0.8 | 1.2 | 0.6 | 15.2 |
| Chlorine content/mg/kg | 3.12 | 2.23 | 3.41 | 2.89 | 50.6 |
| Water content/%) | 0.06 | 0.07 | 0.06 | 0.05 | 0.06 |
| Mechanical impurities/%) | 0.013 | 0.007 | 0.015 | 0.008 | 0.012 |
From the experimental data in table 2, it can be found that the content of metal, scale and chlorine in the fatty acid after the conventional process treatment is far higher than the content of the corresponding substances in the product after the process treatment disclosed in the application, and the fatty acid prepared by the method has low content of metal and phosphorus and low content of chlorine, so that the method is an ideal pretreatment method for the waste oil with high chlorine content.
Claims (10)
1. A pretreatment method of waste oil with high chlorine content comprises the following steps:
a process: waste animal and vegetable fat → adsorption → hydrolysis → continuous drying or continuous distillation;
or
And the process B comprises the following steps: waste animal and vegetable fat → acid treatment → liquid separation → drying → adsorption → hydrolysis → continuous drying or continuous distillation.
2. The method for pretreating waste oil and fat with high chlorine content according to claim 1, wherein the method comprises the following steps: sampling and detecting the discarded animal and vegetable oil, and adopting a process A when the chlorine content is more than or equal to 10mg/kg, the total metal content is less than or equal to 100mg/kg, and the phosphorus content is less than or equal to 10 mg/kg;
sampling and detecting the discarded animal and vegetable oil, and adopting the process B when the chlorine content is more than or equal to 10mg/kg, the total metal content is more than 100mg/kg or the phosphorus content is more than 10 mg/kg.
3. The method for pretreating waste oil and fat with high chlorine content according to claim 1 or 2, wherein the method comprises the following steps: the waste animal and vegetable oil is one or more of waste cooking oil, swill oil, palmitic acid oil, coconut oil and palm oil.
4. The method for pretreating waste oil and fat with high chlorine content according to claim 1 or 2, wherein the method comprises the following steps: in the process B, the acid treatment comprises the following steps: adding 50-85 wt.% acid aqueous solution into the waste animal and vegetable oil for acid treatment, controlling the temperature to be 60-80 ℃, and controlling the acid treatment time to be 30-60 min;
the acid is phosphoric acid or citric acid; the water solution of the acid accounts for 1 to 15 percent of the mass of the waste animal and vegetable oil.
5. The method for pretreating waste oil and fat with high chlorine content according to claim 1 or 2, wherein the method comprises the following steps: in the process B, the liquid separation step is carried out under the conditions as follows: controlling the temperature of the material to be 60-80 ℃, standing for 0.5-6 h, keeping the temperature of the material to be 60-80 ℃, performing oil-water separation, and separating liquid to remove wastewater.
6. The method for pretreating waste oil and fat with high chlorine content according to claim 1 or 2, wherein the method comprises the following steps: in the process B, the drying step is carried out under the following conditions: drying at 90-105 deg.C under 50-100mbar until the water content is not more than 0.5 Wt.%.
7. The method for pretreating fats of waste oil containing high chlorine according to claim 1 or 2, wherein: the adsorption step comprises: adding adsorbent for adsorption at 90-120 deg.C for 10-60min, and filtering after adsorption;
the addition amount of the adsorbent accounts for 0.5-4% of the mass of the waste animal and vegetable oil or the waste animal and vegetable oil after acid treatment, liquid separation and drying.
8. The method for pretreating waste oil and fat with high chlorine content according to claim 7, wherein the method comprises the following steps: the adsorbent is one or a mixture of more of acid clay, activated carbon and silica gel.
9. The method for pretreating waste oil and fat with high chlorine content according to claim 1 or 2, wherein the method comprises the following steps: the hydrolysis step comprises: performing hydrolysis by adopting a medium-high pressure hydrolysis process, and removing generated glycerol after the hydrolysis is finished;
the medium-high pressure hydrolysis process conditions are as follows: the mass ratio of oil to water is 10: 1-1: 1, the reaction pressure is 2.5-5.5 MPa, the reaction temperature is 230-255 ℃, the reaction time is 1-8h, and the hydrolysis rate reaches more than 98%.
10. The method for pretreating waste oil and fat with high chlorine content according to claim 1 or 2, wherein the method comprises the following steps: the continuous drying or continuous distillation step:
sampling and hydrolyzing the obtained material, testing, and continuously drying when the total content of the metal and the phosphorus is less than 30 mg/kg; when the total content of the metal and phosphorus is more than or equal to 30mg/kg, carrying out continuous distillation;
the continuous drying conditions are as follows: vacuum degree of 5-50mbar, retention time of 20-60min, and temperature of 90-110 deg.C;
the continuous distillation conditions were: vacuum degree of 5-50mbar, retention time of 20-60min, temperature of 230-.
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| WO2023235924A1 (en) * | 2022-06-09 | 2023-12-14 | Peerless Holdings Pty Limited | Pre-treatment of waste material for biofuel production |
| CN117801881A (en) * | 2024-02-26 | 2024-04-02 | 北京海新能源科技股份有限公司 | Pretreatment method for waste grease |
| WO2024074759A1 (en) * | 2022-10-03 | 2024-04-11 | Neste Oyj | Process for removal of chloride containing compounds and other impurities from fats and oils |
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