Summary of the invention
For solving the problems of the technologies described above, the present invention proposes a kind of working method of continuous production list bis-fatty acid glyceryl ester, can reach production efficiency height and the stable effect of final product quality through this method.
For achieving the above object, technical scheme of the present invention is following:
A kind of working method of continuous production list bis-fatty acid glyceryl ester comprises:
The proportion relation of reaction mass is set, and said reaction mass comprises glycerine, grease class material and catalyzer; With the said reaction mass preheating that configures, and feed reaction kettle step by step, the control reaction mass carries out the reaction of certain hour at a certain temperature, obtains finished product; The direct output of said finished product is carried out heat exchange with said reaction mass, accomplish once cooling.
Preferably, also comprise with once the cooling after said finished product carry out reducing temperature twice.
Preferably, the said reaction kettle that feeds step by step comprises and feeds the third order reaction still step by step.
Preferably, said grease class material is an animal-plant oil, the triglyceride of saturated or undersaturated condition.
Preferably, said catalyzer is that basic catalyst comprises sodium hydroxide, calcium hydroxide or sodium hydride.
Preferably, the said proportion relation that reaction mass is set comprises the throughput ratio that reaction mass is set.
Preferably, said throughput ratio is: the winterized stearin flow of glycerine flow=(15-30%), the catalyst flow=glycerine (0.1-1%) and the total flux of winterized stearin.
Preferably, said certain temperature is 180-250 ℃.
Preferably, said certain hour is 1-3 hour.
Pass through technique scheme; The working method of continuous production list bis-fatty acid glyceryl ester provided by the present invention is through designing the proportion relation of reaction mass in advance; According to the injected volume of the proportion relation that designs control material, and the main part of reaction is designed to multi-stage reacting kettle carries out successive reaction, can be according to the liquid surface height controlling reaction times of reaction kettle; The drawable reaction kettle of finished product that obtains after the reaction simultaneously cools off; Make whole plant carry out successive production, avoided moving the situation of resting that is caused for chilled product needs arrestment in single still reaction pattern, guaranteed the continuity of producing according to preset proportion relation; Guarantee the stability of quality product simultaneously, and improved production efficiency.
Embodiment
The present invention proposes a kind of working method of continuous production list bis-fatty acid glyceryl ester, can reach production efficiency height and the stable effect of final product quality through this method.
In the present invention, described grease class material comprises that lipid acid consists of each quasi-grease of LAURIC ACID 99 MIN, palmitinic acid, Triple Pressed Stearic Acid, oleic acid and linolic acid etc., can be the saturated product after the hydrogenation, also can be product behind the unhydrogenation.In the embodiment of the invention, preferably use winterized stearin.
Described catalyzer can be an an acidic catalyst; It also can be basic catalyst; Described an acidic catalyst can be StNa, lipid acid etc.; Said basic catalyst for example is sodium hydroxide, calcium hydroxide, Pottasium Hydroxide, potassium hydride KH, sodium hydride etc., and the embodiment of the invention is preferably used sodium hydroxide.
In working method provided by the present invention, need the proportioning of pre-configured reaction mass, said reaction mass comprises glycerine, grease and catalyzer; Said proportioning comprises mass ratio or throughput ratio etc., and the present invention measures through throughput ratio, generally speaking; The flow-ratio control of grease and glycerine exists: the winterized stearin flow of glycerine flow=(15-30%); Be preferably the grease flow of glycerine flow=(20-25%), the difference that catalyst consumption is used according to catalyzer and different, generally speaking; The glycerine and the greasy total flux of catalyst consumption=(0.1-1%); So reaction mass before charging, needs to control earlier the flow of winterized stearin and glycerine, calculate the flow of catalyzer then according to the total flux of grease and glycerine.
Single bis-fatty acid glyceryl ester that the present invention produced is meant the single bis-fatty acid glyceryl ester of content of monoglyceride between 30-60%; Single bis-fatty acid glyceryl ester for different content; The proportioning of reaction mass is different, when for example reaction mass is winterized stearin, glycerine and sodium hydroxide:
Produce 30% single bi-tristearin, required proportioning is: winterized stearin, glycerine, sodium hydroxide proportioning=1: (0.15-0.25): (0.0001-0.002);
Produce 40% single bi-tristearin, required proportioning is: winterized stearin, glycerine, sodium hydroxide proportioning=1: (0.17-0.27) (0.0001-0.002);
Produce 50% single bi-tristearin, required proportioning is: winterized stearin, glycerine, sodium hydroxide proportioning=1: (0.19-0.29): (0.0001-0.002);
Produce 60% single bi-tristearin, required proportioning is: winterized stearin, glycerine, sodium hydride proportioning=1: (0.21-0.30): (0.0001-0.002).
Above-mentioned reaction mass needs controlled temperature at 180-250 ℃ when reacting, and is preferably 200-230 ℃, more preferably 220 ℃; The reaction times of above-mentioned reaction mass is 1-3 hour, is preferably 1.5-2.5 hour, more preferably 2 hours.
The equipment of employed realization continuous production list bis-fatty acid glyceryl ester working method can be equipment as shown in Figure 1 among the present invention; And be not limited to following equipment; For those of ordinary skills, under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to this equipment accompanying drawing; To this, should not cause any qualification of the present invention.
See also Fig. 1; This equipment comprises: preparing tank 11, be used to dispose the catalyzer concentration sodium hydroxide, and through adding a little grease sodium hydroxide is disperseed; And in preparing tank, carry out high-speed stirring; Make it even, preparing tank 11 is connected with a volume pump 12, through the flow of volume pump 12 control catalyst.Reaction mass glycerine and grease carry out flow control through under meter 13, get into preheater 14 with catalyzer jointly according to certain throughput ratio and carry out preheating, and preheater has bilayer structure, comprise pipe layer 141 and shell 142, and reaction mass is flowed through and managed layer 141.Preheater 14 is connected with the third order reaction still, is respectively first step reaction kettle 15, second stage reaction kettle 16 and third stage reaction kettle 17, carries out material through the pump housing 18 between each reaction kettle and pumps.Reaction kettles wherein at different levels inside is provided with three layers of reaction chamber 19; Each reaction chamber 19 is separated by through dividing plate 20; Material in each reaction chamber flows to lower floor's reaction chamber through the space between transmission shaft 21 and the dividing plate 20; Be provided with agitating vane 22 in each layer reaction chamber 19, guarantee that reaction mass reacts fully.Reaction mass obtains reacted finished product behind third stage reaction kettle 17; This finished product is delivered to shell 142 inside of preheater 14 through the pump housing, carries out heat exchange with pipe layer 141 an inner reaction mass, and finished product is once lowered the temperature; Also for reaction volume provides thermal source, practiced thrift the energy simultaneously.Once continue the to flow through interchanger 23 that links to each other with preheater 14 of the finished product after the cooling carries out reducing temperature twice and cools off.
Reaction kettles at different levels bottom also is provided with inlet mouth 24, is used for to control its inner vacuum tightness, guaranteeing carrying out smoothly of reaction kettle internal-response to the inner shielding gas that feeds of reaction kettle.This shielding gas can be a rare gas element, like nitrogen, can also be dioxide gas etc.; It will be appreciated by those skilled in the art that; Except that feeding shielding gas, can also use to vacuumize or vacuumize and realize with feeding the mode that shielding gas combines, this present invention is not done qualification.
Need to prove that the design demand of third order reaction still satisfies certain requirement, enable to guarantee that material residence time in reaction kettle after getting into reaction kettle is not less than 1-3 hour.The said residence time is meant the time of reaction mass complete reaction in reaction kettle, and the ratio calculation through reaction kettle total inventory and final finished flow obtains, and therefore, the height of reaction kettle and the ratio of width need satisfy its design requirements.According to above-mentioned saying, the structure of the reaction kettle that meets design requirement is not limited to structure listed in the present embodiment accompanying drawing, can also be other structures, and to this, the present invention does not do qualification.
The working method of the continuous production list bis-fatty acid glyceryl ester that the embodiment of the invention provided can be implemented through following manner.
At first design the proportion relation of glycerine, grease and sodium hydroxide, and carry out regulating and controlling through system.
Its proportion relation is difference according to producing the different single bis-fatty acid glyceryl ester of content of monoglyceride.Generally speaking, the production content of monoglyceride is single bi-tristearin of 30%, and required proportioning is: grease, glycerine, sodium hydroxide proportioning=1: (0.15-0.25): (0.0001-0.002);
The production content of monoglyceride is single bi-tristearin of 40%, and required proportioning is: winterized stearin, glycerine, sodium hydroxide proportioning=1: (0.17-0.27) (0.0001-0.002);
The production content of monoglyceride is single bi-tristearin of 50%, and required proportioning is: winterized stearin, glycerine, sodium hydroxide proportioning=1: (0.19-0.29): (0.0001-0.002);
The production content of monoglyceride is single bi-tristearin of 60%, and required proportioning is: winterized stearin, glycerine, sodium hydride proportioning=1: (0.21-0.30): (0.0001-0.002).
Then, the reaction mass that configures is fed preheater carry out preheating, the temperature of preheating is 180-250 ℃.
Reaction mass after the preheating is fed the third order reaction still react, temperature of reaction is controlled at 180-250 ℃, is preferably 200-230 ℃, and more preferably 220 ℃, controlling reaction time is 1-3 hour, is preferably 1.5-2.5 hour, more preferably 2 hours.
Finished product feeding preheater and raw material that reaction is obtained carry out heat exchange, and finished product is once lowered the temperature.
Product after once lowering the temperature is fed interchanger carry out the reducing temperature twice cooling, equipment can be proceeded work in the process of cooling of product, need not to stop, and has realized continuous production.
Below, embodiments of the invention are described.
Embodiment one
Present embodiment is that the production content of monoglyceride is single bi-tristearin of 50%, and catalyzer is preferably calcium hydroxide.The operation steps of present embodiment is following:
1, the proportion relation of design reaction mass;
Design winterized stearin feed rate is 2400Kg/h, and the glycerine feed flow is 600Kg/h, the feed rate 0.3Kg/h of calcium hydroxide, and the concentration of the calcium hydroxide-winterized stearin of configuration is 1% (mass ratio of calcium hydroxide and winterized stearin).In preparing tank, put into 200Kg winterized stearin and 2Kg calcium hydroxide, mix well through in preparing tank, carrying out high-speed stirring, the feed rate of adjusting catalyzer according to volume pump is 30Kg/h.
2, reaction mass being fed preheater preheats;
3, the reaction mass after will preheating feeds the third order reaction still and reacts, and control reaction temperature is 200-230 ℃, and the reaction times is 3 hours;
4, reacted finished product is directly fed preheater and reaction mass carries out heat exchange, realize once cooling;
5, the product after will once lowering the temperature feeds interchanger and carries out the reducing temperature twice cooling, and in the product temperature-fall period, this complete equipment can continuous service, feeds intake according to the proportion relation of reaction mass, realizes the continuous production of product.
Embodiment two
Present embodiment is that the production content of monoglyceride is single bi-tristearin of 40%, and catalyzer is preferably sodium hydroxide.The operation steps of present embodiment is following:
1, the proportion relation of design reaction mass;
Design winterized stearin feed rate is 1600Kg/h, and the glycerine feed flow is 400Kg/h, the feed rate 3Kg/h of sodium hydroxide, and the concentration of the sodium hydroxide-winterized stearin of the configuration of configuration is 1% (mass ratio of sodium hydroxide and winterized stearin).In preparing tank, put into 300Kg winterized stearin and 9Kg sodium hydroxide, mix well through in preparing tank, carrying out high-speed stirring, the feed rate of adjusting catalyzer according to volume pump is 100Kg/h.
2, reaction mass being fed preheater preheats;
3, the reaction mass after will preheating feeds the third order reaction still and reacts, and control reaction temperature is 200-230 ℃, and the reaction times is 2 hours;
4, reacted finished product is directly fed preheater and reaction mass carries out heat exchange, realize once cooling;
5, the product after will once lowering the temperature feeds interchanger and carries out the reducing temperature twice cooling, and in the product temperature-fall period, this complete equipment can continuous service, feeds intake according to the proportion relation of reaction mass, realizes the continuous production of product.
Pass through technique scheme; The working method of continuous production list bis-fatty acid glyceryl ester provided by the present invention is through designing the proportion relation of reaction mass in advance; According to the injected volume of the proportion relation that designs control material, and the main part of reaction is designed to multi-stage reacting kettle carries out successive reaction, can be according to the liquid surface height controlling reaction times of reaction kettle; The drawable reaction kettle of finished product that obtains after the reaction simultaneously cools off; Make whole plant carry out successive production, avoided moving the situation of resting that is caused for chilled product needs arrestment in single still reaction pattern, guaranteed the continuity of producing according to preset proportion relation; Guarantee the stability of quality product simultaneously, and improved production efficiency.
Simultaneously, the present invention carries out heat exchange with resulting product and reaction mass, and the temperature of product is reduced, and also for the required temperature of reaction mass certain thermal source is provided.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be conspicuous concerning those skilled in the art, and defined General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments among this paper.Therefore, the present invention will can not be restricted to these embodiment shown in this paper, but will meet and principle disclosed herein and features of novelty the wideest corresponding to scope.