WO2022155775A1 - Système et procédé de production de glycérol raffiné par raffinage de glycérol brut - Google Patents

Système et procédé de production de glycérol raffiné par raffinage de glycérol brut Download PDF

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WO2022155775A1
WO2022155775A1 PCT/CN2021/072655 CN2021072655W WO2022155775A1 WO 2022155775 A1 WO2022155775 A1 WO 2022155775A1 CN 2021072655 W CN2021072655 W CN 2021072655W WO 2022155775 A1 WO2022155775 A1 WO 2022155775A1
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glycerin
tank
crude
condenser
crude glycerin
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PCT/CN2021/072655
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English (en)
Chinese (zh)
Inventor
张新合
滕磊
周焕恩
彭卫星
宋西祥
张书星
周杰
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汇智工程科技股份有限公司
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Priority to PCT/CN2021/072655 priority Critical patent/WO2022155775A1/fr
Publication of WO2022155775A1 publication Critical patent/WO2022155775A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/88—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C31/00—Saturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
    • C07C31/18—Polyhydroxylic acyclic alcohols
    • C07C31/22—Trihydroxylic alcohols, e.g. glycerol

Definitions

  • the invention relates to the technical field of refined glycerin production, in particular to a system and a process for refining and producing refined glycerin from crude glycerin.
  • the technical problem to be solved by the present invention is: to overcome the deficiencies of the prior art, and to provide a system and process for refining crude glycerin to produce refined glycerin, which can refine crude glycerin with a content of 50%-90wt% to obtain a crude glycerol with a content of 95%-99.5%.
  • the wt% of refined glycerin can meet the quality requirements of industrial-grade refined glycerin, resulting in greater social and economic benefits.
  • the present invention provides a system for refining crude glycerin to produce refined glycerin, comprising a crude glycerin pretreatment unit, a crude glycerol distillation and refining unit, and a decolorization and deodorization unit; Crude glycerin pretreatment tank, oil-water separation device, alkali adjusting tank and flash distillation still; the crude glycerin distillation and refining unit comprises a distillation still, a first condenser, a second condenser, a third condenser, a first Four condensers and a fifth condenser; a first heating coil is arranged in the still, a steam pipe is connected to the discharge pipe at the bottom of the still, and the inlet of the still is connected with the crude glycerin outlet of the flash still through pipes; The condensing temperatures of the first condenser, the second condenser, the third condenser, the fourth condenser and the
  • Fraction receiving tank; the decolorizing and deodorizing unit includes a decolorizing kettle, a filter and a temporary storage tank connected in sequence through pipelines, and the inlet of the decolorizing kettle is connected with the fraction outlet of the first fraction receiving tank through pipelines.
  • a second heating coil and an air flotation coil are laid on the bottom surface of the crude glycerin pretreatment tank, and both ends of the second heating coil extend out of the crude glycerin pretreatment tank, respectively.
  • the air inlet of the floating coil is connected with the air outlet of the compressed air buffer tank through a pipeline, and the part of the air floating coil located in the crude glycerin pretreatment tank is provided with several air holes; the lower part of the crude glycerin pretreatment tank is provided with a discharge It also includes an acid tank, the acid tank is provided with an acid inlet pipe and an acid outlet pipe, and the acid outlet pipe extends into the crude glycerin pretreatment tank.
  • the crude glycerol pretreatment unit further includes a crude glycerin preheater, and the crude glycerol preheater is provided with a crude glycerin inlet pipe, a crude glycerol outlet pipe, a heating medium inlet pipe and a heating medium outlet pipe, and the crude glycerin outlet pipe is provided
  • the tube extends into the crude glycerol pretreatment tank.
  • the heating medium inlet pipe and the heating medium outlet pipe are respectively provided with valves
  • the crude glycerin outlet pipe is provided with a first temperature sensor
  • the valve and the first temperature sensor are respectively electrically connected to the controller.
  • the crude glycerol pretreatment tank is provided with a second temperature sensor, and the second temperature sensor is electrically connected to the controller.
  • the oil-water separation device includes an automatic crude glycerin oil separation tank and an oil separation tank; one end of the crude glycerin automatic oil separation tank is provided with a feeding port, and the other end is provided with a feeding port, and the feeding port is provided at the other end.
  • a grease outlet is arranged above the feed port, and the feed port of the crude glycerin automatic oil separation tank is connected with the discharge pipe of the crude glycerol pretreatment tank; in the crude glycerol automatic oil separation tank, several vertical glycerol flow directions are arranged vertically in sequence.
  • each baffle group includes an upper baffle and a lower baffle arranged before and after; there is a gap between the bottom of the upper baffle and the bottom of the crude glycerin automatic oil separation tank, and the bottom of the lower baffle is fixed on the crude glycerin automatic separation tank. There is a gap between the bottom of the oil tank and the top of the lower baffle and the top of the crude glycerin automatic oil separation tank; the top of the oil separation tank is provided with a feed port, the bottom is provided with a discharge port, and the upper part is located at a distance from the feed port.
  • a grease outlet is arranged on the same side of the baffle, and the discharge port of the crude glycerin automatic oil separation tank is connected with the feed port of the oil separation tank through a pipeline; There are gaps with the top of the oil trap and between the bottom of the baffle and the bottom of the oil trap, or the top and bottom of the baffle are respectively provided with openings.
  • a flash heat exchanger is also connected through a pipeline between the alkali conditioning tank and the flash tank.
  • a flash kettle condenser is connected to the steam outlet of the flash kettle through a pipeline, and a water tank is connected to the water outlet of the flash kettle condenser through a pipeline.
  • a hydrocyclone is connected to the upper part of the still, and a desalination tank is connected to the lower part.
  • a vapor-liquid balance tank is connected to the lower part of the distillation still.
  • a second heat exchanger is connected between the flash still and the still through a pipeline.
  • the fraction outlet of the second fraction receiving tank is connected to the inlet of the flash tank through a pipeline, and the fraction outlets of the third fraction receiving tank and the fourth fraction receiving tank are connected to the waste water treatment device through pipelines connect.
  • the crude glycerin distillation and refining unit further includes a steam drum, the air outlet of the cooling medium shell side of the first condenser is connected to the air inlet of the steam drum through a pipeline, and the air outlet of the steam drum is distributed with the steam through a pipeline
  • the liquid inlet of the steam drum is connected to the water supply tank of the steam drum through a pipeline, and the liquid outlet of the steam drum is connected to the liquid inlet of the cooling medium shell side of the first condenser through a pipeline.
  • a liquid level sensor is provided on the steam drum
  • a pump is provided on the pipeline between the steam drum and the water replenishing tank of the steam drum, and the liquid level sensor and the pump are respectively electrically connected to the controller.
  • the glycerin recovery outlet of the filter is connected with the inlet of the decolorization kettle through a pipeline.
  • the present invention also provides a kind of technology that utilizes above-mentioned crude glycerol refining to produce refined glycerin system to produce refined glycerin, comprising the following operations:
  • Crude glycerin pretreatment process the crude glycerin stored in the tank area is pumped into the crude glycerin pretreatment tank, and acid is added to the crude glycerin pretreatment tank, and the crude glycerin is heated and mixed under the action of acid.
  • the hydrolysis reaction occurs, and then the initial separation of fatty acid and crude glycerin is realized under the action of the air flotation coil and the oil-water separation device;
  • the crude glycerin after separating the oil is pumped into the alkali adjustment tank, and the alkali is added to the alkali adjustment tank to adjust the pH. value;
  • the crude glycerin treated with alkali adjustment is pumped to the flash tank for vacuum flash evaporation to remove moisture;
  • the fraction of the first fraction receiving tank is pumped into the decolorization kettle, the activated carbon powder is added to the decolorization kettle, the glycerin enters the filter after stirring, decolorization and adsorption, and the filtered refined glycerin is pumped to In the temporary storage tank, the refined glycerin in the temporary storage tank is pumped to the refined glycerin tank farm.
  • the crude glycerol pretreatment process of step (1) before the crude glycerol is pumped to the crude glycerol pretreatment tank, it is preheated, and the preheating temperature is 50-120°C.
  • the pH value is adjusted to 3.5-6.5 after adding acid to the crude glycerol pretreatment tank.
  • the heating temperature of the crude glycerol pretreatment tank is 80-110°C.
  • the pH value is adjusted to 7-12.
  • step (1) before the crude glycerol after alkali adjustment is pumped to the flash tank, it is first pumped to the flash heat exchanger for heat exchange, and the crude glycerol after heat exchange
  • the temperature is 100-150°C.
  • the pressure of the flash tank is -0.050 to -0.085MPa.
  • the water content of the crude glycerol after flash evaporation is 0.1%-5wt%.
  • step (2) crude glycerol distillation and refining process
  • the crude glycerol after flash dehydration is pumped to the still, it is first pumped to the second heat exchanger for heat exchange, and the temperature after heat exchange is 120-160 °C °C.
  • the distillation temperature of the still is 160-210° C.
  • the pressure of the still is -0.090 to -0.099 MPa.
  • the condensation outlet temperature of the first condenser is 140-200°C
  • the condensation outlet temperature of the second condenser is 110-150°C
  • the condensation outlet temperature of the third condenser is 140-200°C. 50-120°C
  • the condensation outlet temperature of the fourth condenser is 30-60°C
  • the condensation outlet temperature of the fifth condenser is 15-40°C.
  • the fraction in the second fraction receiving tank is returned to the flash tank in the step (1) crude glycerol pretreatment process, and the third fraction receiving tank and the fourth fraction receive The fraction in the tank is sent to the wastewater treatment unit for treatment.
  • the temperature of the decolorization kettle is 50-100°C.
  • the amount of activated carbon powder added is 0.1-0.5wt% of the fraction in the first fraction receiving tank.
  • the stirring and decolorization adsorption time of the decolorization kettle is 1-4h.
  • step (3) before the glycerin in the decolorization kettle enters the filter, sampling and filtration chromaticity detection is performed first, and the detected chromaticity reaches 15-50 and the glycerin content is greater than or equal to 95% before entering the filter. .
  • the filter adopts a plate and frame filter press, a candle filter or a leaf filter.
  • the filtration pressure of the filter is 0.05-0.5MPa.
  • the glycerin in the filter is first passed into the air to empty the filter to the decolorization kettle, and then steam and compressed air are respectively introduced to purge the filter cake, Dry for 20-60min, then open the slag discharge valve at the bottom of the filter to remove the filter cake. After the removal, the filter is restored and the next cycle of filtration is performed until the material in the decolorization kettle is filtered, and the refined glycerin pump in the temporary storage tank Sent to the refined glycerin tank farm.
  • the present invention has the following beneficial effects:
  • the present invention first adopts acidification air flotation to separate and remove the oily impurities such as most of oil, fatty acid and fatty acid methyl ester in the crude glycerin, and then by adjusting the alkali, the remaining small amount of fatty acid in the crude glycerin becomes fatty acid salt, and is converted into reorganization. Phase separation to reduce steaming out, thereby improving the quality of refined glycerin products. Subsequently, the pretreated crude glycerin enters the vacuum still for distillation. During the distillation process, the high-boiling components remain in the still and are separated from the crude glycerol, while the low-boiling components become glycerol and water vapor after gasification.
  • the mixed gas of the main body uses the difference of the boiling points of glycerol and water to obtain semi-finished refined glycerin with different contents and mixtures of glycerol and water with different contents through five-stage condensation.
  • the semi-finished refined glycerin is deodorized, decolorized and filtered by activated carbon powder, and the crude glycerin with a content of 50%-90wt% is refined to obtain refined glycerin with a content of 95%-99.5wt%, which meets the quality requirements of industrial-grade refined glycerin and produces Greater social and economic benefits.
  • part of the glycerin is returned to the distillation kettle for re-distillation to recover the glycerin, and part of it is used as a preparation solution to adjust the content of refined glycerin; the low-concentration glycerol and water mixture is sent to the wastewater treatment plant for treatment. .
  • the present invention adopts kettle-type vacuum distillation, which reduces energy consumption compared with tower-type rectification, and the vacuum degree and heating type (heating coil and direct steam heating) of the distillation still of the present invention can turn over the material in the still. , to prevent the scaling of the heating coil, and to reduce the boiling point of the system through the addition of water vapor, which is convenient for distillation and increases production capacity.
  • Figure 1 is a schematic diagram of the connection of the crude glycerol pretreatment unit of the present invention.
  • Fig. 2 is the connection schematic diagram of the crude glycerin distillation and refining unit and the decolorization and deodorization unit of the present invention.
  • FIG. 3 is a process flow diagram of the present invention.
  • FIG. 4 is a schematic structural diagram of a crude glycerin pretreatment tank, a crude glycerin preheater and an acid tank of the present invention.
  • FIG. 5 is a schematic structural diagram of the oil-water separation device of the present invention.
  • FIG. 6 is a schematic structural diagram of the steam drum of the present invention.
  • 100-crude glycerin pretreatment unit 200-crude glycerin distillation and refining unit, 300-decolorization and deodorization unit, 101-crude glycerin pretreatment tank, 10101-second heating coil, 10102-air flotation coil, 102 - Crude glycerin automatic oil separation tank, 10201-upper partition, 10202-lower partition, 103-oil separator, 10301-partition plate, 104-alkali adjustment tank, 105-flash kettle, 106-crude glycerin preheater , 10601-crude glycerin inlet pipe, 10602-crude glycerin outlet pipe, 10603-heating medium inlet pipe, 10604-heating medium outlet pipe, 107-flash heat exchanger, 108-compressed air buffer tank, 109-acid tank, 10901 -acid inlet pipe, 10902-acid outlet pipe, 110-first temperature sensor, 111-second temperature sensor
  • the present embodiment provides a system for refining crude glycerin to produce refined glycerin, including a crude glycerin pretreatment unit 100, a crude glycerin distillation and refining unit 200, and a decolorization and deodorization unit 300;
  • the processing unit 100 includes a crude glycerin pretreatment tank 101, an oil-water separation device, an alkali adjustment tank 104 and a flash distillation kettle 105 connected in sequence through pipelines, and a flash evaporation heat exchange is also connected between the alkali adjustment tank 104 and the flash distillation kettle 105 through pipelines.
  • the crude glycerin distillation and refining unit 200 includes a distillation still 201, a first condenser 202, a second condenser 203, a third condenser 204, a fourth condenser 205 and a fifth condenser 206 connected in sequence through pipes
  • a second heat exchanger is connected between the flash still 105 and the still 201 through a pipeline
  • the still 201 is provided with a first heating coil 20101, the upper part of the still 201 is connected with a hydrocyclone 211, and the lower part is connected with a
  • the desalination tank and the vapor-liquid balance tank 212, the discharge pipe at the bottom of the still 201 is connected with a steam pipe 20102, and the inlet of the still 201 is connected with the crude glycerin outlet of the flash still 105 through pipes;
  • the fraction receiving tank 207 and the fraction outlet of the third condenser 204 are connected to the second fraction receiving tank 208 through pipelines, the fraction outlet of the fourth condenser 205 is connected to the third fraction receiving tank 209 through pipelines, and the fractions of the fifth condenser 206
  • the outlet is connected with a fourth fraction receiving tank 210 through a pipeline;
  • the decolorization and deodorization unit 300 includes a decolorization kettle 301, a filter 302 and a temporary storage tank 303 connected in turn through a pipeline, and the glycerin recovery outlet of the filter 302 is connected with the decolorization kettle 301.
  • the inlet is connected by a pipeline
  • the inlet of the decolorization kettle 301 is connected with the fraction outlet of the first fraction receiving tank 207 respectively by a pipeline
  • the fraction outlet of the second fraction receiving tank 208 is connected with the inlet of the flash kettle 105 by a pipeline
  • the third fraction receiving tank is connected by a pipeline.
  • 209 and the distillate outlet of the fourth distillate receiving tank 210 are connected to the waste water treatment device through pipes.
  • the bottom surface of the crude glycerin pretreatment tank 101 is laid with a second heating coil 10101 and an air flotation coil 10102, and both ends of the second heating coil 10101 extend out of the crude glycerin pretreatment tank 101 respectively.
  • the air inlet of the air flotation coil 10102 is connected to the air outlet of the compressed air buffer tank 108 through a pipeline, and the part of the air flotation coil 10102 located in the crude glycerin pretreatment tank 101 is provided with several air holes;
  • the lower part of the tank 101 is provided with a discharge pipe 115; it also includes an acid tank 109, the acid tank 109 is provided with an acid inlet pipe 10901 and an acid outlet pipe 10902, and the acid outlet pipe 10902 extends into the crude glycerin pretreatment tank 101.
  • the crude glycerin pretreatment unit 100 further includes a crude glycerin preheater 106, and the crude glycerin preheater 106 is provided with a crude glycerin inlet pipe 10601, a crude glycerol outlet pipe 10602, a heating medium inlet pipe 10603 and a heating medium outlet pipe 10604. , the crude glycerol outlet pipe 10602 extends into the crude glycerol pretreatment tank 101 .
  • the heating medium inlet pipe 10603 and the heating medium outlet pipe 10604 are respectively provided with a valve 114, and the crude glycerin outlet pipe 10602 is provided with a first temperature sensor 110, the valve 114 and the first temperature sensor 110 are respectively electrically connected with the controller,
  • the first temperature sensor 110 monitors the temperature of the preheated crude glycerin, thereby controlling the preheating of the crude glycerol by the heating medium through the valve 114, and finally automatically controls the preheated temperature of the crude glycerin to meet the production requirements.
  • the crude glycerin pretreatment tank 101 is provided with a second temperature sensor 111, the second temperature sensor 111 is electrically connected to the controller, and the second temperature sensor 111 can monitor the temperature in the crude glycerol pretreatment tank 101 in real time, and adjust the The valve 114 on the heating coil 10101 adjusts the temperature in the crude glycerol pretreatment tank 101 to ensure that the hydrolysis temperature is maintained at 80-110°C.
  • the oil-water separation device includes an automatic crude glycerin oil separation tank 102 and an oil separation tank 103; one end of the crude glycerin automatic oil separation tank 102 is provided with a feed port, and the other end is provided with a discharge port, A grease outlet is arranged above the feeding port, and the feeding port of the crude glycerin automatic oil separation tank 102 is connected with the discharge pipe 115 of the crude glycerin pretreatment tank 101; the crude glycerin automatic oil separation tank 102 is vertically vertical in sequence along the flow direction of the crude glycerin.
  • each baffle group includes an upper baffle 10201 and a lower baffle 10202 arranged before and after; there is a gap between the bottom of the upper baffle 10201 and the bottom of the crude glycerin automatic oil separation tank 102, and the lower baffle
  • the bottom of the plate 10202 is fixed at the bottom of the crude glycerin automatic oil separation tank 102 and there is a gap between the top of the lower baffle 10202 and the top of the crude glycerol automatic oil separation tank 102;
  • the top of the oil separation tank 103 is provided with a feeding port, and the bottom A discharge port is provided, the upper part and the feed port are located on the same side of the baffle plate 10301, and a grease outlet is provided, and the discharge port of the crude glycerin automatic oil separation tank 102 is connected with the feed port of the oil separation tank 103 through a pipeline;
  • the A baffle plate 10301 is vertically arranged in the oil trap tank 103 , and there are gaps or barriers between the
  • the crude glycerol distillation and refining unit 200 also includes a steam drum 213.
  • the air outlet of the cooling medium shell side of the first condenser 202 is connected to the air inlet of the steam drum 213 through a pipeline, and the air outlet of the steam drum 213 is connected to the steam drum 213 through a pipeline.
  • the steam distribution table 214 is connected; the liquid inlet of the steam drum 213 is connected to the steam drum replenishment tank 215 through a pipeline, and the liquid outlet of the steam drum 213 is connected to the liquid inlet of the cooling medium shell side of the first condenser 202 through a pipeline.
  • the steam drum 213 is provided with a liquid level sensor 216, and the pipeline between the steam drum 213 and the steam drum replenishment tank 215 is provided with a pump 217.
  • the liquid level sensor 216 and the pump are respectively electrically connected to the controller.
  • the crude glycerin stored in the tank area is pumped to the crude glycerin preheater 106 to be preheated to 80°C, and the preheated crude glycerol is pumped to the crude glycerol pretreatment tank 101, and the crude glycerol is pretreated through the acid tank 109.
  • Add acid may be hydrochloric acid, sulfuric acid or organic acid
  • Add acid may be hydrochloric acid, sulfuric acid or organic acid
  • the tank 101 adjusts the pH value to 3.5-6.5; at the same time pass the high temperature steam into the crude glycerin pretreatment tank 101 through the second heating coil 10101, and heat it to 100 ° C, and the compressed air is introduced into the air flotation coil 10102 through the compressed air buffer tank 108, and the compressed air is discharged from the air hole on the air flotation coil 10102 into the crude glycerin pretreatment tank 101 to form micro-bubbles, thereby in acid
  • the crude glycerin is heated and air-mixed under the action of
  • the fatty acid-based compounds in crude glycerin are hydrolyzed to obtain fatty acids, which are separated from the glycerol-water mixture under the action of micro-bubble air flotation (fatty acids have low density and float on the upper layer).
  • the crude glycerin after acidification hydrolysis and air flotation oil separation treatment is transported to the crude glycerin automatic oil separation tank 102 by a pump, and the fatty acid and crude glycerin are separated layer by layer by several upper baffles 10201 and lower baffles 10202, and finally Because fatty acid and crude glycerol have a large density difference (density of fatty acid is 0.9g/ml, crude glycerol is 1.2g/ml), the liquid level at one end of the feed port of crude glycerol automatic oil separator 102 is higher than that at the end of the discharge port. The liquid level is high, and the higher part is the fatty acid layer. This part of the automatically separated fatty acids will automatically flow out through the grease outlet and be transported to the grease collection tank, thereby realizing the automatic separation of fatty acids and crude glycerol.
  • the crude glycerin that flows out from the discharge port of the crude glycerin automatic oil separation tank 102 still contains a small amount of fatty acids, and after entering the grease trap 103, the fatty acids with less density will float on the upper layer of the liquid level of the grease trap 103, and are removed from the oil trap 103.
  • the grease outlet of the grease trap 103 flows out and is transported to the grease collection tank, so as to further remove the crude glycerin; and the crude glycerin in the lower layer will pass through the gap between the bottom of the baffle 10301 and the bottom of the grease trap 103 or
  • the opening at the bottom of the baffle plate 10301 flows into the other end of the baffle plate 10301, and is finally pumped out from the discharge port at the bottom of the baffle plate 10301 to the alkali adjusting tank 104 for the next step; the top of the baffle plate 10301 and the oil separator
  • the gaps between the tops of the tanks 103 or the openings at the tops of the baffles 10301 are for gas phase balance in the oil traps 103 .
  • Using the oil-water separation device of this embodiment can remove more than 95% of fatty acids in the process of pretreatment and oil separation.
  • the crude glycerin after separating the grease is pumped into the alkali adjusting tank 104, and an alkaline substance (can be sodium hydroxide, potassium hydroxide or calcium hydroxide) is added to the alkali adjusting tank 104, and the pH value is adjusted to 7-12.
  • the remaining trace fatty acids in the glycerol are neutralized to generate fatty acid sodium salts, which are converted into high-boiling components, and finally discharged as the residual liquid of the flash tank 105 in the subsequent process, thereby reducing the impact on the quality of refined glycerin.
  • the crude glycerin treated with alkali adjustment is pumped to the flash heat exchanger 107 for heat exchange, and the temperature of the crude glycerol after heat exchange is 120 ° C, and then pumped to the flash tank 105 for vacuum flash evaporation to remove moisture.
  • the pressure of the flash still 105 is -0.065 ⁇ -0.080MPa
  • the water content of the crude glycerin after the flash is 1wt%
  • the steam after the flash enters the flash still condenser 112 and condenses into a liquid phase and is collected in the water tank 113.
  • the crude glycerol after the flash dehydration is pumped to the second heat exchanger for heat exchange, and the crude glycerol temperature after the heat exchange is 120-130 ° C; 205°C, the pressure of the autoclave is -0.090 ⁇ -0.099MPa.
  • high-boiling components and salt remain in still still 201, and finally discharge still 201 as raffinate, and the crystalline solid salt produced in the partial distillation process is collected by the desalting tank at the bottom of still 201 and then discharged from still 201.
  • the vapor-liquid balance tank 212 at the bottom of the still 201 plays the role of high-temperature superheated water vapor-liquid separation and heat recovery: the steam entering the still 201 is medium-pressure steam, and the condensed water temperature is very high (180-210 ° C, pressure > 20 kg) , the system fluctuation will cause secondary gasification to affect heat exchange.
  • the condensed water enters the vapor-liquid balance tank 212 the vaporized steam enters the distillation still 201 again through the upper riser for heat exchange.
  • the superheated water in the vapor-liquid balance tank 212 Then it enters the lower-level feed heat exchanger and reuses the heat of the superheated water.
  • the steam pipe 20102 on the discharge pipe 115 at the bottom of the still 201 can play the role of dredging and heating the valve of the lower discharge pipe.
  • the gas phase distilled from the distillation still 201 undergoes five-stage condensation successively.
  • the first condenser 202 condenses the 140-200 °C fraction into the first fraction receiving tank 207
  • the second condenser 203 condenses the 110-150 °C fraction into the first fraction receiving tank 207.
  • Fraction receiving tank 207, the third condenser 204 condenses the fraction at 50-120 °C into the second fraction receiving tank 208, the fourth condenser 205 condenses the fraction at 30-60 °C and enters the third fraction receiving tank 209, the fifth condensing
  • the 15-40° C. fraction condensed from the device 206 enters the fourth fraction receiving tank 210 .
  • what the first fraction receiving tank 207 collects is a fraction with high glycerol content (glycerol content ⁇ 95wt%), which enters into the subsequent decolorization and deodorization process;
  • what the second fraction receiving tank 208 collects is a fraction with low glycerin content (glycerol content be 10-40wt%), return to the flash tank 105 in the crude glycerin pretreatment process, to reclaim the glycerin therein;
  • the third fraction receiving tank 209 collects waste water with ultra-low glycerol content (the glycerol content is 0-5wt %), the fourth fraction receiving tank 210 collects waste water and low boilers, and the third fraction receiving tank 209 and the fourth fraction receiving tank 210 collect fractions together into the wastewater treatment device for treatment.
  • the first condenser 202 condenses and recovers the fraction at 140-200° C.
  • the high-temperature crude glycerin gas phase in the tube side of the first condenser 202 exchanges heat with the shell-side hot water, part of the hot water vaporizes into steam at a high temperature, which Part of the steam contains thermal energy and should be recycled.
  • a steam drum 213 is added on the side of the shell side of the cooling medium of the first condenser 202, and the low-pressure waste heat steam generated by the high temperature gasification of the water phase in the shell side of the cooling medium of the first condenser 202 first enters through the pipeline In the steam drum 213, and finally into the steam distribution table 214, it can be used for the preheating of crude glycerin at room temperature, the temperature adjustment of the crude glycerin pretreatment tank 101, the temperature adjustment of the decolorization kettle 301, and the flash dehydration and other devices.
  • the steam drum 213 is replenished with water through the steam drum replenishment tank 215, and the water in the steam drum 213 is replenished to the shell side through the pipeline connected to the shell side of the first condenser 202, so that The continuous cycle is carried out to condense the high boiling point glycerol in the gas phase tube side of the first condenser 202, and the low boiling point gas phase such as uncondensed water vapor enters the subsequent stage condenser.
  • the fraction collected by the first fraction receiving tank 207 is pumped into the decolorizing still 301, under the cooperation of steam and circulating water, the temperature of the decolorizing still 301 is 80 °C, and the activated carbon powder is added to the decolorizing still 301, and the amount of the activated carbon powder is added. It is 0.25 wt % of the fraction in the first fraction receiving tank 207 .
  • the filter 302 can be a plate and frame filter press, a candle filter 302 or a leaf filter 302, and the filter pressure of the filter 302 is 0.2-0.4MPa.
  • the impurities and activated carbon powder in the filtrate gradually decrease until it is qualified.
  • the filter layer becomes thick and saturated, the filtration pressure increases, and the filtrate becomes At this time, it should be switched to the filter cake unloading procedure: first, the glycerin in the filter 302 is discharged to the decolorization kettle 301 by passing air, and then steam and compressed air are respectively introduced to purge and dry the filter cake for 20-60min, and then Open the slag discharge valve at the bottom of the filter 302 to remove the filter cake.
  • the filter 302 is restored and the next cycle of filtration is performed until the material in the decolorizing kettle 301 is filtered, and the refined glycerin in the temporary storage tank 303 is pumped to the Refined glycerin tank farm.
  • the glycerin content is 97 wt % and the chromaticity is 30.
  • Embodiment 1 This embodiment is the same as Embodiment 1, except that:
  • the crude glycerin stored in the tank farm is pumped to the preheater to be preheated to 60°C; the heating temperature of the crude glycerol pretreatment tank 101 is 80°C; the crude glycerol after alkali adjustment is pumped to the flash heat exchanger 107 Heat exchange is carried out in the heat exchange, and the temperature of the crude glycerin after heat exchange is 100° C.; the pressure of the flash tank 105 is -0.050 ⁇ -0.070MPa, and the water content of the crude glycerol after flash evaporation is 3wt%.
  • the crude glycerol after flash dehydration is pumped to the second heat exchanger for heat exchange, and the temperature of the crude glycerol after heat exchange is 150°C; the distillation temperature of the still 201 is 180-200°C.
  • the temperature of the decolorization kettle 301 is 50°C; the amount of activated carbon powder added is 0.1 wt % of the fractions of the first condenser 202 and the second condenser 203; the time for glycerin stirring, decolorization and adsorption is 1 hour; the filtration pressure of the filter 302 is 0.15 -0.25MPa.
  • the glycerin content is 96 wt % and the chromaticity is 40.
  • Embodiment 1 This embodiment is the same as Embodiment 1, except that:
  • the crude glycerin stored in the tank farm is pumped to the preheater to be preheated to 100°C; the heating temperature of the crude glycerin pretreatment tank 101 is 110°C; the crude glycerol after alkali adjustment is pumped to the flash heat exchanger 107 Heat exchange is carried out in the middle, and the crude glycerin temperature after heat exchange is 140° C.; the pressure of the flash tank 105 is -0.070 ⁇ -0.085MPa, and the water content of the crude glycerol after flash evaporation is 0.1wt%.
  • the crude glycerol after flash dehydration is pumped to the second heat exchanger for heat exchange, and the temperature of the crude glycerol after heat exchange is 150-160°C; the distillation temperature of the still 201 is 190-210°C.
  • the temperature of the decolorization kettle 301 is 100°C; the amount of activated carbon powder added is 0.5 wt % of the fractions of the first condenser 202 and the second condenser 203; the time for glycerin stirring, decolorization and adsorption is 4 hours; the filtration pressure of the filter 302 is 0.3 -0.45MPa.
  • the glycerin content is 99.5 wt % and the chromaticity is 20.
  • Embodiment 1 This embodiment is the same as Embodiment 1, except that:
  • the crude glycerin stored in the tank farm is pumped to the preheater to be preheated to 50°C; the heating temperature of the crude glycerin pretreatment tank 101 is 90°C; the crude glycerol after alkali adjustment is pumped to the flash heat exchanger 107 Heat exchange is carried out in the middle, and the temperature of the crude glycerin after heat exchange is 150° C.; the pressure of the flash tank 105 is -0.050 ⁇ -0.065MPa, and the water content of the crude glycerol after flash evaporation is 5wt%.
  • the crude glycerin after flash evaporation and dehydration is pumped to the second heat exchanger for heat exchange, and the temperature of the crude glycerol after heat exchange is 130-140°C; the distillation temperature of the still 201 is 160-180°C.
  • the temperature of the decolorizing kettle 301 is 60°C; the amount of activated carbon powder added is 0.3 wt % of the fractions of the first condenser 202 and the second condenser 203; the time for stirring, decolorizing and adsorbing glycerin is 3 hours; the filtration pressure of the filter 302 is 0.05 -0.15MPa.
  • the glycerin content is 95 wt % and the chromaticity is 30.
  • Embodiment 1 This embodiment is the same as Embodiment 1, except that:
  • the crude glycerin stored in the tank farm is pumped to the preheater to be preheated to 120°C; the heating temperature of the crude glycerin pretreatment tank 101 is 85°C; the crude glycerol after alkali adjustment is pumped to the flash heat exchanger 107 Heat exchange is carried out in the heat exchange, and the temperature of the crude glycerin after heat exchange is 110° C.; the pressure of the flash tank 105 is -0.070 ⁇ -0.085MPa, and the water content of the crude glycerol after flash evaporation is 2wt%.
  • the crude glycerin after flash dehydration is pumped to the second heat exchanger for heat exchange, and the temperature of the crude glycerol after heat exchange is 140-150°C; the distillation temperature of the still 201 is 170-190°C.
  • the temperature of the decolorizing kettle 301 is 70°C; the amount of activated carbon powder added is 0.4 wt % of the fractions of the first condenser 202 and the second condenser 203; the time for stirring, decolorizing and adsorbing glycerin is 2 hours; the filtration pressure of the filter 302 is 0.40 -0.50MPa.
  • the glycerin content is 98 wt % and the chromaticity is 50.
  • Embodiment 1 This embodiment is the same as Embodiment 1, except that:
  • the crude glycerol after steaming and dehydration is pumped to the second heat exchanger for heat exchange, and the temperature of the crude glycerol after heat exchange is 110°C; the distillation temperature of the still 201 is 150-159°C.
  • the glycerin content is 93 wt % and the chromaticity is 30.
  • This comparative example is the same as Example 1, except that:
  • the temperature of the decolorization kettle 301 is 110° C.; the amount of activated carbon powder added is 0.05 wt % of the fractions of the first condenser 202 and the second condenser 203; the time for glycerin stirring, decolorization and adsorption is 3 hours; the filtration pressure of the filter 302 is 0.35 -0.40MPa.
  • the glycerin content is 98.5 wt % and the chromaticity is 80.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

L'invention concerne un système et un procédé de production de glycérol raffiné par raffinage de glycérol brut, se rapportant au domaine technique de la production de glycérol raffiné. La solution technique selon la présente invention porte sur : un système qui comprend une unité de prétraitement de glycérol brut, une unité de raffinage de distillation de glycérol brut et une unité de décoloration et de désodorisation. Selon la présente invention, du glycérol brut ayant une teneur de 50 à 90 % en poids peut être raffiné pour obtenir du glycérol raffiné ayant une teneur de 95 à 99,5 % en poids, qui répond aux exigences de qualité du glycérol raffiné de qualité industrielle et génère de grands avantages socioéconomiques.
PCT/CN2021/072655 2021-01-19 2021-01-19 Système et procédé de production de glycérol raffiné par raffinage de glycérol brut WO2022155775A1 (fr)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090198088A1 (en) * 2008-02-01 2009-08-06 Lanxess Sybron Chemicals Inc. Process for the purification of crude glycerin utilizing ion exclusion chromatorgraphy and glycerin concentration
CN103965019A (zh) * 2014-04-04 2014-08-06 天长市康宁塑胶科技有限公司 一种甘油的纯化生产工艺
CN104262098A (zh) * 2013-12-11 2015-01-07 宁波杰森绿色能源科技有限公司 一种生物柴油副产品粗甘油的综合利用方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090198088A1 (en) * 2008-02-01 2009-08-06 Lanxess Sybron Chemicals Inc. Process for the purification of crude glycerin utilizing ion exclusion chromatorgraphy and glycerin concentration
CN104262098A (zh) * 2013-12-11 2015-01-07 宁波杰森绿色能源科技有限公司 一种生物柴油副产品粗甘油的综合利用方法
CN103965019A (zh) * 2014-04-04 2014-08-06 天长市康宁塑胶科技有限公司 一种甘油的纯化生产工艺

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"HANDBOOK OF LIGHT INDUSTRY TECHNICAL EQUIPMENT", vol. 4, 31 December 1996, CHINA NATIONAL LIGHT INDUSTRY COUNCIL, article CHINA NATIONAL LIGHT INDUSTRY COUNCIL: "Glycerin Distillation Device)" *

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