CN201750964U - Glycerin distillation device - Google Patents

Glycerin distillation device Download PDF

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Publication number
CN201750964U
CN201750964U CN2010202602883U CN201020260288U CN201750964U CN 201750964 U CN201750964 U CN 201750964U CN 2010202602883 U CN2010202602883 U CN 2010202602883U CN 201020260288 U CN201020260288 U CN 201020260288U CN 201750964 U CN201750964 U CN 201750964U
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CN
China
Prior art keywords
tower
distillation
glycerine
tower section
joint
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
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CN2010202602883U
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Chinese (zh)
Inventor
郭学阳
张中法
丁爱梅
黄慧
吕彩玲
温占平
李津哲
张景龙
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WEIFANG ZHONGYE CHEMICAL CO Ltd
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WEIFANG ZHONGYE CHEMICAL CO Ltd
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Priority to CN2010202602883U priority Critical patent/CN201750964U/en
Application granted granted Critical
Publication of CN201750964U publication Critical patent/CN201750964U/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The utility model discloses a glycerin distillation device, comprising a thin film evaporator, a distillation tower, a condenser and a backflow receiving tank, which are communicated in order. The distillation tower comprises a lower tower section, a middle tower section and an upper tower section which are arranged from down to top, wherein the lower tower section is provided with a silk screen therein, and the middle tower section and the upper tower section are respectively equipped with filling materials therein. The glycerin distillation device of the utility model combines the thin film evaporation and the conventional distillation and adopts the semi-continuous processing to carry out the operation, reducing the production energy consumption and the distillation residue, increasing the product purity and decreasing the product impurity. The product purity reaches over 99.5% (GC) and the product impurity content is less than or equal to 0.5% (GC), satisfying the quality requirement of the pharmaceutical or cosmetic grade and expanding the product application field.

Description

A kind of glycerol distillation device
Technical field
The utility model relates to the chemical industry equipment field, relates in particular to a kind of glycerol distillation device.
Background technology
Glycerine has another name called glycerine, being mainly used in industries such as medicine, cosmetics, alkyd resins, food, beverage, polyurethanes, celluloid, explosive, paint, weaving, papermaking, tobacco, textile printing and dyeing, is indispensable chemicals in industry, medicine, national defence and the daily life.The source of glycerine, the one, the accessory substance of soap industry, the 2nd, make with extraordinary culture propagation molasses, be that to be that raw material is synthetic with the propylene make in addition.The quality quality of glycerine directly influences its application and market value, and wherein distillation process has directly determined the final mass of finished product glycerine.The crude glycerine distillation equipment of present domestic use is according to the mode difference, and three kinds of air-cooled type, water-cooled and thin-film distillations are arranged.
1, glycerine air-cooled type distillation: air-cooled type is generally lined up two stringers by 8 empty garden tubes, with the most of glycerine of water condensation, 1 empty garden tube and 3 shell and tube condenser condensation sugar water.
2, glycerol liquor cold type distillation: water-cooled is mainly three shell and tube condensers, and first condenser cools off with crude glycerine, two, three condenser water coolings.
3, glycerine thin-film distillation: the glycerine thin-film distillation is to make crude glycerine form the shaped liquid film flash evaporation under certain vacuum and temperature, the time that stops in pot than steam distillation crude glycerine shortens greatly, it is overheated and the loss of the glycerine that causes is significantly improved the smell of distillation glycerine to prevent and reduce glycerine.
In the still-process of glycerine, the loss of glycerine is mainly: the air flue loss of uncooled glycerine, fail to steam clean residue equal loss at the bottom of the polymerization of glycerine, decomposition and the distillation still.Wherein the type of the design of distillation equipment and selection, destilling tower and internal structure, reflux ratio determine etc. bigger to influences such as product quality, yield and economic benefits.Although existing various distilling apparatus has advantage separately, but still have following deficiency: (1) product glycerine has color, purity is low, contains impurity such as polymerization glycerine: (2) use simple distillation or to not further investigation of distil process, single complete equipment production capacity is low; (3) distillation equipment selects for use (comprising feed entrance point, distillation still or heating facility, destilling tower type and internal structure design etc.) improper or improper to the backflow position of the return line when of refluxing, and causes the product production capacity low, of poor benefits.
In recent years, along with glycerine is more and more as the amount that byproduct produces in preparation biodiesel process, also more deep thereupon to the utilization research of glycerine.Transformation of glycerol becomes chemical intermediates such as propane diols, ethylene glycol and chloropropylene oxide, and glycerine is used for animal feed has entered large-scale production; Make glycerine and hcl reaction generate the new technology industrialization of epoxychloropropane, have tangible resource, safety, cost and investment advantage with respect to propylene high-temperature chloridising and propylene acetate method; Producing of many uses, important chemical material, medicine intermediate and food additives dihydroxyacetone (DHA) (DHA) with glycerine for the fermenting raw materials method succeeds.The deep processed product of above-mentioned glycerine, indexs such as the purity of glycerine, impurity have been proposed more harsh requirement, reinforcement is to the research of glycerol distillation technology and equipment, design more reasonable, energy-conservation, as to improve glycerine purity distilling apparatus, for glycerine and deep processing industry development thereof with increase the benefit, meaning is remarkable.
Summary of the invention
Technical problem to be solved in the utility model is: the deficiency at prior art exists provides a kind of product purity height, yield height and energy consumption low glycerol distillation device.
For solving the problems of the technologies described above, the technical solution of the utility model is:
A kind of glycerol distillation device, described distilling apparatus comprises thin film evaporator, destilling tower, condenser and the backflow receiving tank that order is communicated with, described destilling tower comprises bottom Ta Jie, middle part tower joint and the upper column joint that is provided with from bottom to top, described bottom Ta Jienei is provided with silk screen, is respectively equipped with filler in described middle part tower joint and the upper column joint.
As a kind of improvement, described upper column joint and middle part tower joint are respectively equipped with tower return line and middle tower return line, and are communicated with the bottom of described backflow receiving tank.
As further improvement, described upper column joint is respectively equipped with different fillers with middle part Ta Jienei.
As further improving, described bottom Ta Jie is provided with hand hole again.
The top of described backflow receiving tank is provided with vacuum interface.
Owing to adopted technique scheme, the beneficial effects of the utility model are:
1, the utility model is used in combination thin film evaporator and destilling tower, form semi-continuous distillation technology, both advantages are got up, not only reduced the heated time of glycerine in the still-process, reduce the growing amount of polymerization glycerine in the still-process and glycerine because of chemical reactions such as oxidation change the amount of other products into, improved product appearance, and distillation efficiency improves greatly, improved the production capacity of single device.
2, the utility model adopts dual reflux to regulate the material composition of gas-liquid two-phase, under the constant situation of feed rate, two return valve apertures of last tower return line and middle tower return line are constant, reflux ratio is basicly stable, adopt half-continuous process to operate, constant product quality, and effectively improved the purity of distillage, product purity reaches more than 99.5% (GC), reduced bottoms, reduced product impurity, product impurity content≤0.5% (GC), reach pharmaceutical grade or cosmetics-stage quality requirement, enlarged the application of product.
3, the utility model employing decompression operation, so vapo(u)rizing temperature reduces than prior art, greatly reduces energy consumption, can the loss-rate prior art reduce more than 5%, reduce production cost, and significantly reduced the oxidation of glycerine and the growing amount of polymerization glycerine, improved product purity.
4, the bottom Ta Jie of the utility model destilling tower is provided with the foam removal silk screen, the foam of carrying secretly in the steam can be become drop and return thin film evaporator and distill once more, is provided with hand hole at bottom Ta Jie in addition, is convenient to the filling and the taking-up of silk screen.
5, upper column of the present utility model joint and middle part tower joint are equipped with the filler of unlike material, dissimilar, different specific areas respectively, help the abundant contact and the mass transfer of gas, liquid two-phase, make finished product glycerine keep higher concentration.
Description of drawings
Below in conjunction with drawings and Examples the utility model is further specified.
Accompanying drawing is the structural representation of the utility model embodiment.
Among the figure, 1. thin film evaporator; 2. destilling tower; 21. bottom Ta Jie; 22. middle part tower joint; 23. upper column joint; 24. silk screen; 25. middle part filler; 26. top filler; 27. hand hole; 3. condenser; 4. backflow receiving tank; 41. refluxing opening; 42. vacuum interface; 43. product outlet; 5. go up the tower return line; 6. middle tower return line.
The specific embodiment
As shown in drawings, a kind of glycerol distillation device, described distilling apparatus comprises thin film evaporator 1, destilling tower 2, condenser 3 and the backflow receiving tank 4 that order is communicated with, described destilling tower 2 comprises bottom Ta Jie 21, middle part tower joint 22 and the upper column joint 23 that is provided with from bottom to top, be provided with silk screen 24 in the described bottom Ta Jie 21, the sidewall of described bottom Ta Jie 21 is provided with hand hole 27.Be respectively equipped with middle part filler 25 and top filler 26 in described middle part tower joint 22 and the upper column joint 23.Described upper column joint 23 and middle part tower joint 22 are respectively equipped with tower return line 5 and middle tower return line 6, and are communicated with the refluxing opening 41 of backflow receiving tank 4 bottoms.
During the utility model work, the vacuum interface 42 of opening backflow receiving tank 4 is communicated with vacuum system, production is carried out under vacuum condition, after treating rate of air sucked in required and vacustat, add crude glycerine continuously to the thin film evaporator 1 that feeds heat medium, after making crude glycerine in thin film evaporator 1, heat vaporization, enter destilling tower 2, at first through bottom Ta Jie 21, after becoming the foam of carrying secretly in the steam into drop, silk screen 24 in the bottom Ta Jie 21 turns back to thin film evaporator 1, distill vaporization once more, remove the steam that defoams and enter middle part tower joint 22 and upper column joint 23, steam is in the process that bottom Ta Jie 21 rises to upper column joint 23, and the component that boiling point is higher than glycerine is fewer and feweri, glycerine purity constantly increases, and the solution-air two-phase is at middle part tower joint 22, vaporization-condensation between the upper column joint 23 is carried out repeatedly.Early stage is when operating, the valve opening of last tower return line 5 is surpassed 2/3, the valve opening of middle tower return line 6 surpasses 1/2, when glycerol content in the backflow receiving tank 4 surpasses 99% (GC), turn down the valve opening of tower return line 5, when glycerol content in the backflow receiving tank 4 reaches 99.5% (GC) when above, keep, in the valve opening of two return lines constant, regulate the temperature and the flow of heat medium this moment, control the flow that adds crude glycerine in the thin film evaporator 1 well, under stable state of the art, distill, the finished product glycerol content that enters backflow receiving tank 4 remains unchanged substantially, purity remains on more than 99.5% (GC), and the product that reaches quality requirement discharges the finished product receiving tank from the product outlet 43 of the receiving tank 4 that refluxes.
The material of upper column of the present utility model joint 23 and middle part tower joint 22 top fillers 26 that are equipped with and middle part filler 27 is different, type difference, specific area difference, helps the abundant contact and the mass transfer of solution-air two-phase, makes finished product glycerine keep higher concentration.The utility model is provided with hand hole 27 at bottom Ta Jie 21 in addition, is convenient to the filling and the taking-up of silk screen 24.

Claims (5)

1. glycerol distillation device, it is characterized in that: described distilling apparatus comprises thin film evaporator, destilling tower, condenser and the backflow receiving tank that order is communicated with, described destilling tower comprises bottom Ta Jie, middle part tower joint and the upper column joint that is provided with from bottom to top, described bottom Ta Jienei is provided with silk screen, is respectively equipped with filler in described middle part tower joint and the upper column joint.
2. glycerol distillation device as claimed in claim 1 is characterized in that: described upper column joint and middle part tower joint are respectively equipped with tower return line and middle tower return line, and are communicated with the bottom of described backflow receiving tank.
3. glycerol distillation device as claimed in claim 1 is characterized in that: described upper column joint is respectively equipped with different fillers with middle part Ta Jienei.
4. glycerol distillation device as claimed in claim 1 is characterized in that: described bottom Ta Jie is provided with hand hole.
5. as claim 1,2,3 or 4 described glycerol distillation devices, it is characterized in that: the top of described backflow receiving tank is provided with vacuum interface.
CN2010202602883U 2010-07-16 2010-07-16 Glycerin distillation device Expired - Fee Related CN201750964U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2010202602883U CN201750964U (en) 2010-07-16 2010-07-16 Glycerin distillation device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2010202602883U CN201750964U (en) 2010-07-16 2010-07-16 Glycerin distillation device

Publications (1)

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CN201750964U true CN201750964U (en) 2011-02-23

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CN2010202602883U Expired - Fee Related CN201750964U (en) 2010-07-16 2010-07-16 Glycerin distillation device

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CN (1) CN201750964U (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103263780A (en) * 2013-05-22 2013-08-28 华南理工大学 Film filler evaporator
CN104707353A (en) * 2015-02-12 2015-06-17 浙江华诺化工有限公司 Glycerin distillation system
CN111957062A (en) * 2020-09-11 2020-11-20 赵汇川 Reduced pressure distillation device and process for continuous desalting of crude glycerol

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103263780A (en) * 2013-05-22 2013-08-28 华南理工大学 Film filler evaporator
CN104707353A (en) * 2015-02-12 2015-06-17 浙江华诺化工有限公司 Glycerin distillation system
CN111957062A (en) * 2020-09-11 2020-11-20 赵汇川 Reduced pressure distillation device and process for continuous desalting of crude glycerol

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GR01 Patent grant
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20110223

Termination date: 20120716