CN102417865A - Method for continuously producing mono-and-di-glyceride - Google Patents

Method for continuously producing mono-and-di-glyceride Download PDF

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CN102417865A
CN102417865A CN2010102947205A CN201010294720A CN102417865A CN 102417865 A CN102417865 A CN 102417865A CN 2010102947205 A CN2010102947205 A CN 2010102947205A CN 201010294720 A CN201010294720 A CN 201010294720A CN 102417865 A CN102417865 A CN 102417865A
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reaction
fatty acid
continuous production
glyceryl ester
working method
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CN102417865B (en
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陈小龙
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Zhangjiagang Zhongding Additives Co ltd
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CHINA TOP CHEMICAL (JIANGSU) Co Ltd
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Abstract

The invention discloses a method for continuously producing mono-and-di-glyceride. The method comprises the following steps of: setting the ratio relation of reaction materials comprising glycerin, a grease substance and a catalyst; preheating the prepared reaction materials, injecting the preheated materials in a reaction kettle stepwise, controlling the reaction materials to perform a reaction at a certain temperature for a certain time and obtain the finished product; and directly outputting the finished product to perform heat exchange with the reaction materials, and cooling for one time. By adopting the method provided by the invention, continuous production can be realized and the effects of high production efficiency and stable finished product quality can be realized.

Description

The working method of continuous production list bis-fatty acid glyceryl ester
Technical field
The present invention relates to the working method of single bis-fatty acid glyceryl ester, be specifically related to a kind of working method of continuous production list bis-fatty acid glyceryl ester.
Background technology
Single bis-fatty acid glyceryl ester generally is meant the single bis-fatty acid glyceryl ester of content of monoglyceride between 30-60%.In the current techniques, manufacture order bis-fatty acid glyceryl ester mainly is to realize i.e. direct esterification method and alcoholysis method through two kinds of methods.Said direct esterification method is meant lipid acid and glycerine reacted under the situation that catalyzer exists and obtains single bis-fatty acid glyceride product; Said alcoholysis method is to adopt grease and glycerine under the situation that catalyzer exists, to react the single bis-fatty acid glyceride product that obtains.In general, alcoholysis method has some outstanding advantages than the direct esterification method, as: can not produce large quantity of moisture in the course of processing, can avoid reaction process to bubble, and need not be equipped with a large amount of condensation cooling apparatus etc.
Yet; Traditional alcoholysis method all is the production model that adopts single still reaction, when discharging is carried out in the reaction completion, and necessary arrestment; And in still, cool off; Otherwise can cause the equipment wall surface coking owing to the surplus temperature of heating thermal oil is too high, need clean when producing next time, produces a large amount of waste water.
Single still production model can not be carried out successive production, and this discontinuity has also caused the unstable of reaction, for example: need carry out proportioning again to each starting material before each reaction; Proportioning can be because measurement instrument and artificial operation cause labile factor; Simultaneously, also can there be labile factor in processing temperature owing to opertaing device and human factor, moreover; Also can there be labile factor in processing units itself, and various labile factors gather together and cause reacted final product quality unstable.
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.
Description of drawings
Fig. 1 is the equipment synoptic diagram of the working method of the disclosed realization continuous production of embodiment of the invention list bis-fatty acid glyceryl ester.
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.

Claims (9)

1. the working method of a continuous production list bis-fatty acid glyceryl ester is characterized in that, comprising:
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.
2. the working method of continuous production list bis-fatty acid glyceryl ester according to claim 1 is characterized in that, also comprises the said finished product after once lowering the temperature is carried out reducing temperature twice.
3. the working method of continuous production list bis-fatty acid glyceryl ester according to claim 1 and 2 is characterized in that, the said reaction kettle that feeds step by step comprises and feeds the third order reaction still step by step.
4. the working method of continuous production list bis-fatty acid glyceryl ester according to claim 1 and 2 is characterized in that, said grease class material is the triglyceride of animal-plant oil, saturated or undersaturated condition.
5. the working method of continuous production list bis-fatty acid glyceryl ester according to claim 1 and 2 is characterized in that, said catalyzer is that basic catalyst comprises sodium hydroxide, calcium hydroxide or sodium hydride.
6. the working method of continuous production list bis-fatty acid glyceryl ester according to claim 1 is characterized in that the said proportion relation that reaction mass is set comprises the throughput ratio that reaction mass is set.
7. according to the working method of claim 1 or 6 described continuous production list bis-fatty acid glyceryl ester, it is characterized in that 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.
8. the working method of continuous production list bis-fatty acid glyceryl ester according to claim 1 is characterized in that said certain temperature is 180-250 ℃.
9. the working method of continuous production list bis-fatty acid glyceryl ester according to claim 1 is characterized in that said certain hour is 1-3 hour.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104479885A (en) * 2014-11-28 2015-04-01 浙江赞宇科技股份有限公司 Method and device for continuously producing triglyceride
CN105950797A (en) * 2016-07-13 2016-09-21 嘉兴赞宇科技有限公司 Novel preparation process of synthetic fatting agent and device
CN107400564A (en) * 2016-05-19 2017-11-28 嘉兴中诚环保科技股份有限公司 Pipe reaction equipment and continuous esterification method for esterification
CN109678703A (en) * 2019-01-29 2019-04-26 河南工业大学 A kind of synthetic method of monoglyceride
CN114133328A (en) * 2021-10-22 2022-03-04 江苏环宇康力科技有限公司 Production process and formula for preparing monoglyceride from grease

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101575285A (en) * 2009-04-29 2009-11-11 李普选 Technical method for continuously producing fatty glyceride and special equipment thereof
CN201406393Y (en) * 2009-04-29 2010-02-17 李普选 Special device for continuously producing fatty glyceride

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101575285A (en) * 2009-04-29 2009-11-11 李普选 Technical method for continuously producing fatty glyceride and special equipment thereof
CN201406393Y (en) * 2009-04-29 2010-02-17 李普选 Special device for continuously producing fatty glyceride

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104479885A (en) * 2014-11-28 2015-04-01 浙江赞宇科技股份有限公司 Method and device for continuously producing triglyceride
CN107400564A (en) * 2016-05-19 2017-11-28 嘉兴中诚环保科技股份有限公司 Pipe reaction equipment and continuous esterification method for esterification
CN105950797A (en) * 2016-07-13 2016-09-21 嘉兴赞宇科技有限公司 Novel preparation process of synthetic fatting agent and device
CN109678703A (en) * 2019-01-29 2019-04-26 河南工业大学 A kind of synthetic method of monoglyceride
CN109678703B (en) * 2019-01-29 2021-07-13 河南工业大学 Synthetic method of monoglyceride
CN114133328A (en) * 2021-10-22 2022-03-04 江苏环宇康力科技有限公司 Production process and formula for preparing monoglyceride from grease

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Effective date of registration: 20240312

Address after: 215000 West Side of Beijing Road, Jiangsu Yangtze River International Chemical Industry Park, Suzhou City, Jiangsu Province

Patentee after: Zhangjiagang Zhongding Additives Co.,Ltd.

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Address before: 215614 North Road, Xizhang Town, Fenghuang Town, Zhangjiagang City, Suzhou City, Jiangsu Province

Patentee before: CHINA TOP CHEMICAL (JIANGSU) Co.,Ltd.

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