CN204058300U - A kind of high-temperature reflux hydrolysate oil is separated the device preparing glycerine - Google Patents

A kind of high-temperature reflux hydrolysate oil is separated the device preparing glycerine Download PDF

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Publication number
CN204058300U
CN204058300U CN201420331600.1U CN201420331600U CN204058300U CN 204058300 U CN204058300 U CN 204058300U CN 201420331600 U CN201420331600 U CN 201420331600U CN 204058300 U CN204058300 U CN 204058300U
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pipeline
glycerine
tower
vessel
vaporizer
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孔德明
刘佐
陈东伟
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Fengyi oil technology (Dongguan) Co., Ltd.
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Fengyi Oil Chemical (dongguan) Co Ltd
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Abstract

The utility model relates to glycerine technical field, particularly relate to a kind of high-temperature reflux hydrolysate oil and be separated the device preparing glycerine, comprise fat hydrolysis device, sugar water pretreatment unit, glycerol liquor evaporation unit and glycerol distillation device, fat hydrolysis device comprises successively by primary heater that pipeline connects, first degasser, hydrolysis tower, first oil skimmer vessel, first vaporizer, second oil skimmer vessel and sugar water hold-up vessel, sugar water pretreatment unit comprises successively by secondary heater that pipeline connects, mixing tank, 3rd oil skimmer vessel, retort, plate filter, first receiving tank, deep bed filter and the second receiving tank, glycerol liquor evaporation unit comprises successively by the second vaporizer that pipeline connects, glycerol liquor receiving tank and glycerol liquor hold-up vessel, glycerol distillation device comprises successively by the 3rd well heater that pipeline connects, second degasser, distillation tower, glycerine receiving tank, bleaching tower, accurate filter and glycerin storage tank.The utility model can produce stay-in-grade glycerine.

Description

A kind of high-temperature reflux hydrolysate oil is separated the device preparing glycerine
Technical field
The utility model relates to glycerine technical field, particularly relates to a kind of high-temperature reflux hydrolysate oil and is separated the device preparing glycerine.
Background technology
Glycerine, also known as glycerol, is a kind of thick liquid, pleasantly sweet, so be called glycerine, can with water with arbitrarily than miscible, and having strong water absorbability, is important basic organic.1779, Sweden chemist thanked and strangles (Scheele) and accidentally from sweet oil and the reaction of yellow lead oxide, obtain glycerine # this is the existence that people know glycerine for the first time.
The earliest, people are only using the moisturizing agent of glycerine as skin, and to 1846, sieve Sha Boli (Sobrero), by glycerine and nitric acid reaction, obtained nitroglycerine.After 20 years, nitroglycerine and diatomite have been made safety explosive by Nobel, make nitroglycerine successfully can be applied to the production of dynamite.Now, the purposes of glycerine is very extensive, is mainly used in the aspects such as medicine, makeup, Synolac, tobacco, food, beverage, polyurethane(s), zylonite, explosive, textile printing and dyeing.Nearly 1700 multiple uses.
Due to the consumption day by day of the Nonrenewable energy resources such as oil, finding clean renewable energy source becomes chemist obligation one can't decline, glycerine, derives from nature, nontoxic, is desirable industrial chemicals.Therefore, how to develop glycerine well, production equipment and the technique of glycerine become study hotspot.
The production of glycerine mainly adopts fat hydrolysis to obtain, and in prior art, the hydrolysis of grease adopts intermittent type normal pressure catalyzed hydrolytic methods, and the method production cycle is long, and steam loss is large, and percent hydrolysis is lower, and hydrolysis qualities of glycerin is not high.
Summary of the invention
The purpose of this utility model is to provide a kind of high-temperature reflux hydrolysate oil to be separated the device preparing glycerine for the deficiencies in the prior art, and this device percent hydrolysis is high, can produce high quality, stable refining decolouring glycerine.
To achieve these goals, the utility model adopts following technical scheme: a kind of high-temperature reflux hydrolysate oil is separated the device preparing glycerine, comprises fat hydrolysis device, sugar water pretreatment unit, glycerol liquor evaporation unit and glycerol distillation device, fat hydrolysis device comprises successively by primary heater that pipeline connects, first degasser, hydrolysis tower, first oil skimmer vessel, first vaporizer, second oil skimmer vessel and sugar water hold-up vessel, sugar water pretreatment unit comprises successively by secondary heater that pipeline connects, mixing tank, 3rd oil skimmer vessel, retort, plate filter, first receiving tank, deep bed filter and the second receiving tank, secondary heater is connected with sugar water hold-up vessel by pipeline, and glycerol liquor evaporation unit comprises successively by the second vaporizer that pipeline connects, glycerol liquor receiving tank and glycerol liquor hold-up vessel, the second vaporizer is connected with the second receiving tank by pipeline, and glycerol distillation device comprises successively by the 3rd well heater that pipeline connects, second degasser, distillation tower, glycerine receiving tank, bleaching tower, accurate filter and glycerin storage tank, the 3rd well heater is connected with glycerol liquor hold-up vessel by pipeline.
Further, described hydrolysis tower is connected with croude fatty acids tripping device, and croude fatty acids tripping device comprises the 4th well heater, the 3rd degasser and the croude fatty acids hold-up vessel that are connected by pipeline successively, and the 4th well heater is connected with hydrolysis tower by pipeline.
Further, described first vaporizer, between described second vaporizer and described hydrolysis tower, be connected to process water circulation device, process water circulation device comprises the vaporize water receiving tank be connected by pipeline with the first vaporizer, the second vaporizer respectively and the technique water pot be connected by pipeline with vaporize water receiving tank, and technique water pot is connected by pipeline with hydrolysis tower.
Further, described distillation tower is connected with residue treatment device, residue treatment device comprises the residue distillation tower be connected by pipeline with distillation tower and the residue hold-up vessel be connected by pipeline with residue distillation tower, and residue distillation tower is also connected with described second degasser by pipeline.
Further, described primary heater, secondary heater, the 3rd well heater and the 4th well heater are shell and tube heat exchanger.
Further, described first vaporizer is triple-effect evaporator, and described second vaporizer is quadruple effect evaporator.
Further, described hydrolysis tower is high-temperature reflux hydrolysis tower.
Further, described hydrolysis tower is connected with high pressure steam transfer lime, and described technique water pot is connected with process water transfer lime.
Further, described primary heater is connected with material tank by pipeline, and described mixing tank is connected with hydrochloric acid feed pot by pipeline, and described retort is connected with sorbent material loading hopper by pipeline.
Further, described second degasser is connected with liquid caustic soda feed pot by pipeline, and described bleaching tower is connected with gac loading hopper by pipeline.
The beneficial effects of the utility model are: the utility model adopts high pressure-temperature continuous countercurrent hydrolysis method hydrolysate oil to isolate glycerine, percent hydrolysis high (more than 98%), can large scale continuous prod, save the energy, and the concentration of output glycerine sugar water is higher and cleaner; Glycerine sugar water evaporation concentration raw glycerine to 90% under vacuum after impurity elimination purification, then distill under vacuum, through activated carbon adsorption decolouring, obtain the refining decolouring glycerine conformed to quality requirements.
accompanying drawing illustrates:
Fig. 1 is structured flowchart of the present utility model.
Fig. 2 is the structured flowchart of fat hydrolysis device described in the utility model.
Fig. 3 is the structured flowchart of sugar water pretreatment unit described in the utility model.
Fig. 4 is the structured flowchart of glycerol liquor evaporation unit described in the utility model.
Fig. 5 is the structured flowchart of glycerol distillation device described in the utility model.
Reference numeral is: 1-fat hydrolysis device, 11-primary heater, 111-material tank, 12-the first degasser, 13-hydrolysis tower, 131-high pressure steam transfer lime, 14-the first oil skimmer vessel, 15-the first vaporizer, 16-the second oil skimmer vessel, 17-sugar water hold-up vessel, 2-sugar water pretreatment unit, 21 secondary heaters, 22-mixing tank, 221-hydrochloric acid feed pot, 23-the three oil skimmer vessel, 24-retort, 241-sorbent material loading hopper, 25-plate filter, 26-the first receiving tank, 27-deep bed filter, 28-the second receiving tank, 3-glycerol liquor evaporation unit, 31-the second vaporizer, 32-glycerol liquor receiving tank, 33-glycerol liquor hold-up vessel, 4-glycerol distillation device, 41-the three well heater, 42-the second degasser, 421-liquid caustic soda feed pot, 43-distillation tower, 44-glycerine receiving tank, 45-bleaching tower, 451-gac loading hopper, 46-accurate filter, 47-glycerin storage tank, 5-croude fatty acids tripping device, 51-the four well heater, 52-the three degasser, 53-croude fatty acids hold-up vessel, 6-process water circulation device, 61-vaporize water receiving tank, 62-technique water pot, 621-process water transfer lime, 7-residue treatment device, 71-residue distillation tower, 72-residue hold-up vessel.
embodiment:
For the ease of the understanding of those skilled in the art, be further described below in conjunction with embodiment and accompanying drawing 1 ~ 5 pair of the utility model, the content that embodiment is mentioned is not to restriction of the present utility model.
See Fig. 1 ~ 5, a kind of high-temperature reflux hydrolysate oil is separated the device preparing glycerine, comprises fat hydrolysis device 1, sugar water pretreatment unit 2, glycerol liquor evaporation unit 3 and glycerol distillation device 4, fat hydrolysis device 1 comprises the primary heater 11 connected by pipeline successively, first degasser 12, hydrolysis tower 13, first oil skimmer vessel 14, first vaporizer 15, second oil skimmer vessel 16 and sugar water hold-up vessel 17, sugar water pretreatment unit 2 comprises the secondary heater 21 connected by pipeline successively, mixing tank 22, 3rd oil skimmer vessel 23, retort 24, plate filter 25, first receiving tank 26, deep bed filter 27 and the second receiving tank 28, secondary heater 21 is connected with sugar water hold-up vessel 17 by pipeline, and glycerol liquor evaporation unit 3 comprises successively by the second vaporizer 31 that pipeline connects, glycerol liquor receiving tank 32 and glycerol liquor hold-up vessel 33, second vaporizer 31 are connected with the second receiving tank 28 by pipeline, and glycerol distillation device 4 comprises successively by the 3rd well heater 41 that pipeline connects, second degasser 42, distillation tower 43, glycerine receiving tank 44, bleaching tower 45, accurate filter 46 and glycerin storage tank the 47, three well heater 41 are connected with glycerol liquor hold-up vessel 33 by pipeline.
Principle of work of the present utility model is: 1, be hydrolyzed: stock oil is heated to about 105 ~ 115 DEG C through primary heater 11, under the vacuum condition of about 105 ~ 115mBar, air is removed in the first degasser 12, then pump into hydrolysis tower 13 by high-pressure pump from bottom, process water is pumped into from hydrolysis tower 13 top by high-pressure pump.Hydrolysis tower 13 reacts under 45 ~ 55Bar pressure He at 240 ~ 260 DEG C of temperature, stock oil in the way rising to hydrolysis tower 13 top triglyceride level by excessive process water from top to bottom adverse current be hydrolyzed to lipid acid and glycerine.Glycerine sugar water is from hydrolysis tower 13 bottom discharge (concentration about about 15%), through the first oil skimmer vessel 14 skim upper strata impurity, again under vacuum after the first vaporizer 15 is concentrated, concentration can reach 35 ~ 40%, again after impurity removed by the second oil skimmer vessel 16, then pump into sugar water hold-up vessel 17.
2, sugar water pre-treatment: the sugar water of sugar water hold-up vessel 17 gets to workshop by pump, secondary heater 21 is heated to about 75 ~ 85 DEG C by low-pressure steam, enter after mixing tank 22 mixes after the 3rd oil skimmer vessel 23 skim upper strata impurity with mineral acid and enter retort 24, add mineral alkali, inorganic salt are generated with mineral acid neutralization reaction in sugar water, PH is regulated to be 7 ~ 9, add flocculating aids again for forming filter cake at flame filter press, in the material of becoming reconciled filter out by flame filter press the inorganic salt that neutralization reaction generates, and then after being filtered further by deep bed filter 27, then the second receiving tank 28 is pumped into.
3, pre-treatment glycerol liquor evaporation: the pretreated glycerol liquor of the second receiving tank 28 squeezes into workshop through pump, by after the second vaporizer 31 under vacuum condition, in glycerol liquor, the concentration of glycerine is concentrated to about 90% by about 35%, then pumps into glycerol liquor hold-up vessel 33.
4, glycerol distillation and decolouring: the glycerine of glycerol liquor hold-up vessel 33 squeezes into workshop by pump, 85 ~ 95 DEG C are heated to through the 3rd well heater 41, carry out degassed through the second degasser 42 under vacuum, glycerine after degassed pumps into distillation tower 43 and distills, distillation is at high vacuum (<20mBar), carry out at 150 ~ 170 DEG C of temperature, major product distillates in the middle part of distillation tower 43, the purity of glycerine reaches 99.5%, the color and luster of glycerine after bleaching tower 45 of distillation is reduced within 5, again through accurate filter 46, obtain purity more than 99.5%, glycerine within color and luster 5, finally pump into glycerin storage tank 47.
The utility model adopts high pressure-temperature continuous countercurrent hydrolysis method hydrolysate oil to isolate glycerine, percent hydrolysis high (more than 98%), can large scale continuous prod, save the energy, and the concentration of output glycerine sugar water is higher and cleaner; Glycerine sugar water evaporation concentration raw glycerine to 90% under vacuum after impurity elimination purification, then distill under vacuum, through activated carbon adsorption decolouring, obtain the refining decolouring glycerine conformed to quality requirements.
In the present embodiment, described hydrolysis tower 13 is connected with croude fatty acids tripping device 5, croude fatty acids tripping device 5 is comprised the 4th well heater 51, the 3rd degasser 52 and croude fatty acids hold-up vessel the 53, four well heater 51 that are connected by pipeline successively and is connected with hydrolysis tower 13 by pipeline.The croude fatty acids generated floats to tower top based on the difference of proportion, be discharged on the top of hydrolysis tower 13, croude fatty acids the 4th well heater 51 is heated to about 105 ~ 115 DEG C, under the vacuum condition of about 105 ~ 115mBar, degassed in the 3rd degasser 52, then pump into croude fatty acids hold-up vessel 53.
In the present embodiment, described first vaporizer 15, between described second vaporizer 31 and described hydrolysis tower 13, be connected to process water circulation device 6, process water circulation device 6 comprises the vaporize water receiving tank 61 be connected by pipeline with the first vaporizer 15, second vaporizer 31 respectively and the technique water pot 62 be connected by pipeline with vaporize water receiving tank 61, and technique water pot 62 is connected by pipeline with hydrolysis tower 13.The water that sugar water is evaporated is collected through vaporize water receiving tank 61, pumps into technique water pot 62 Recycling after condensation; Collected through vaporize water receiving tank 61 by the moisture evaporated in glycerol liquor, after condensation, pump into technique water pot 62 Recycling.
In the present embodiment, described distillation tower 43 is connected with residue treatment device 7, residue treatment device 7 comprises the residue distillation tower 71 be connected by pipeline with distillation tower 43 and the residue hold-up vessel 72 be connected by pipeline with residue distillation tower 71, and residue distillation tower 71 is also connected with described second degasser 42 by pipeline.When distilling effect is deteriorated, partial material is arranged to residue distillation tower 71 bottom distillation tower 43, residue distillation tower 71 is also at high vacuum (<20mBar), temperature is carried out under 150 ~ 170 DEG C of conditions, the cut that can distill is sent the second degasser 42 back to through pipeline and is continued distillation when raw material, and the residue do not distilled sends into residue hold-up vessel 72.
In the present embodiment, described primary heater 11, secondary heater 21, the 3rd well heater 41 and the 4th well heater 51 are shell and tube heat exchanger.
In the present embodiment, described first vaporizer 15 is triple-effect evaporator, and described second vaporizer 31 is quadruple effect evaporator.
In the present embodiment, described hydrolysis tower 13 is high-temperature reflux hydrolysis tower.
In the present embodiment, described primary heater 11 is connected with material tank 111 by pipeline, and described hydrolysis tower 13 is connected with high pressure steam transfer lime 131, and described technique water pot 62 is connected with process water transfer lime 621.Material tank 111 is for oil of supplying raw materials; High pressure steam transfer lime 131 is for providing the temperature needed for hydrolysis, and temperature is provided by the steam of direct 60 ~ 65Bar; Process water transfer lime 621 is for the process water needed for supplementary hydrolysis.
In the present embodiment, described mixing tank 22 is connected with hydrochloric acid feed pot 221 by pipeline, and described retort 24 is connected with sorbent material loading hopper 241 by pipeline.Hydrochloric acid feed pot 221, for providing hydrochloric acid soln, regulates hydrochloric acid flow to make pH remain on 1.5 ~ 3, and under this pH condition, the acid in sugar water, ester impurities are easily floating; Sorbent material loading hopper 241 is for adding calcium hydroxide and diatomite.
In the present embodiment, described second degasser 42 is connected with liquid caustic soda feed pot 421 by pipeline, and described bleaching tower 45 is connected with gac loading hopper 451 by pipeline.Liquid caustic soda feed pot 421 is for providing sodium hydroxide solution, and gac loading hopper 451 is for adding gac.
Above-described embodiment is the utility model preferably implementation, and in addition, the utility model can also realize by alternate manner, and any apparent replacement is all within protection domain of the present utility model without departing from the concept of the premise utility.

Claims (10)

1. high-temperature reflux hydrolysate oil is separated the device preparing glycerine, it is characterized in that: comprise fat hydrolysis device, sugar water pretreatment unit, glycerol liquor evaporation unit and glycerol distillation device, fat hydrolysis device comprises successively by primary heater that pipeline connects, first degasser, hydrolysis tower, first oil skimmer vessel, first vaporizer, second oil skimmer vessel and sugar water hold-up vessel, sugar water pretreatment unit comprises successively by secondary heater that pipeline connects, mixing tank, 3rd oil skimmer vessel, retort, plate filter, first receiving tank, deep bed filter and the second receiving tank, secondary heater is connected with sugar water hold-up vessel by pipeline, and glycerol liquor evaporation unit comprises successively by the second vaporizer that pipeline connects, glycerol liquor receiving tank and glycerol liquor hold-up vessel, the second vaporizer is connected with the second receiving tank by pipeline, and glycerol distillation device comprises successively by the 3rd well heater that pipeline connects, second degasser, distillation tower, glycerine receiving tank, bleaching tower, accurate filter and glycerin storage tank, the 3rd well heater is connected with glycerol liquor hold-up vessel by pipeline.
2. a kind of high-temperature reflux hydrolysate oil according to claim 1 is separated the device preparing glycerine, it is characterized in that: described hydrolysis tower is connected with croude fatty acids tripping device, croude fatty acids tripping device comprises the 4th well heater, the 3rd degasser and the croude fatty acids hold-up vessel that are connected by pipeline successively, and the 4th well heater is connected with hydrolysis tower by pipeline.
3. a kind of high-temperature reflux hydrolysate oil according to claim 1 is separated the device preparing glycerine, it is characterized in that: described first vaporizer, between described second vaporizer and described hydrolysis tower, be connected to process water circulation device, process water circulation device comprises the vaporize water receiving tank be connected by pipeline with the first vaporizer, the second vaporizer respectively and the technique water pot be connected by pipeline with vaporize water receiving tank, and technique water pot is connected by pipeline with hydrolysis tower.
4. a kind of high-temperature reflux hydrolysate oil according to claim 1 is separated the device preparing glycerine, it is characterized in that: described distillation tower is connected with residue treatment device, residue treatment device comprises the residue distillation tower be connected by pipeline with distillation tower and the residue hold-up vessel be connected by pipeline with residue distillation tower, and residue distillation tower is also connected with described second degasser by pipeline.
5. a kind of high-temperature reflux hydrolysate oil according to claim 2 is separated the device preparing glycerine, it is characterized in that: described primary heater, secondary heater, the 3rd well heater and the 4th well heater are shell and tube heat exchanger.
6. a kind of high-temperature reflux hydrolysate oil according to claim 1 is separated the device preparing glycerine, and it is characterized in that: described first vaporizer is triple-effect evaporator, described second vaporizer is quadruple effect evaporator.
7. a kind of high-temperature reflux hydrolysate oil according to claim 1 is separated the device preparing glycerine, it is characterized in that: described hydrolysis tower is high-temperature reflux hydrolysis tower.
8. a kind of high-temperature reflux hydrolysate oil according to claim 3 is separated the device preparing glycerine, and it is characterized in that: described hydrolysis tower is connected with high pressure steam transfer lime, described technique water pot is connected with process water transfer lime.
9. a kind of high-temperature reflux hydrolysate oil according to claim 1 is separated the device preparing glycerine, it is characterized in that: described primary heater is connected with material tank by pipeline, described mixing tank is connected with hydrochloric acid feed pot by pipeline, and described retort is connected with sorbent material loading hopper by pipeline.
10. a kind of high-temperature reflux hydrolysate oil according to claim 1 is separated the device preparing glycerine, it is characterized in that: described second degasser is connected with liquid caustic soda feed pot by pipeline, and described bleaching tower is connected with gac loading hopper by pipeline.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105255594A (en) * 2015-10-30 2016-01-20 杭州油脂化工有限公司 Grease high-pressure hydrolysis production method and production device by recycling sweet water
CN106495382A (en) * 2016-09-29 2017-03-15 绍兴齐英膜科技有限公司 A kind of processing method of sugar water
CN114854497A (en) * 2022-05-26 2022-08-05 江苏瑞高生物科技有限公司 Device and method for removing free fatty acid from waste vegetable oil
CN115745746A (en) * 2022-07-29 2023-03-07 湖北天基生物能源科技发展有限公司 Glycerol refining method

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105255594A (en) * 2015-10-30 2016-01-20 杭州油脂化工有限公司 Grease high-pressure hydrolysis production method and production device by recycling sweet water
CN106495382A (en) * 2016-09-29 2017-03-15 绍兴齐英膜科技有限公司 A kind of processing method of sugar water
CN106495382B (en) * 2016-09-29 2019-07-16 绍兴齐英膜科技有限公司 A kind of processing method of sugar water
CN114854497A (en) * 2022-05-26 2022-08-05 江苏瑞高生物科技有限公司 Device and method for removing free fatty acid from waste vegetable oil
CN115745746A (en) * 2022-07-29 2023-03-07 湖北天基生物能源科技发展有限公司 Glycerol refining method

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Address after: 523000 New Town Industrial Park, Ma Chung, Dongguan, Guangdong

Patentee after: Fengyi oil technology (Dongguan) Co., Ltd.

Address before: 523147 fengsha oil chemical (Dongguan) Co., Ltd., Xin Sha Industrial Park, Ma Chung, Dongguan, Guangdong

Patentee before: Fengyi oil chemical (Dongguan) Co., Ltd.

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