CN101696155A - Glycerol blackfoot distilling process and glycerol blackfoot distilling still for implementing same - Google Patents
Glycerol blackfoot distilling process and glycerol blackfoot distilling still for implementing same Download PDFInfo
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- CN101696155A CN101696155A CN200910176881A CN200910176881A CN101696155A CN 101696155 A CN101696155 A CN 101696155A CN 200910176881 A CN200910176881 A CN 200910176881A CN 200910176881 A CN200910176881 A CN 200910176881A CN 101696155 A CN101696155 A CN 101696155A
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Abstract
The invention discloses a glycerol blackfoot distilling process, and in particular relates to a process which is to change the glycerol from liquid state to gas state by adopting steam distillation technology on the basis of changing the physical form of the glycerol so as to separate blackfoot impurites and glycerol fundamentally, and separate the glycerol and the blackfoot from different channels in different mass ratio of different forms so as to improve the yield of the glycerol and effectively reduce waste of raw materials. The invention also discloses a glycerol blackfoot distilling still for implementing the process. The distilling still is characterized in that: the lower part of a tower bottom is connected with a heat exchanger which consists of a plurality of independent heating tubes, and open-ended relief pipes which are arranged outside the heating tubes. The glycerol blackfoot distilling still with the arrangement has the advantages of quickly vaporizing the glycerol in a low boiling point state, and improving the working efficiency.
Description
Technical field
Public affairs of the present invention relate to the black pin distil process of a kind of glycerine, are specifically related to a kind of employing vapor distillation technology and realize that isolating glycerine deceives the pin distil process; The invention still further relates to a kind of black pin still kettle of glycerine that realizes this technology.
Background technology
When the industry stearic acid is produced, make the winterized stearin hydrolysis get croude fatty acids, again through the distillation stearic acid that gets product by high pressure-temperature.Can obtain negative product aqueous glycerin solution simultaneously, after its processing, again through concentrating and distill and to produce pure glycerin, the black pin of the continuous discharging of palpus glycerine in still-process, usually the black pin of the glycerine that emits can adopt distillatory method distillation extraction glycerine once more, and resource is utilized fully.And the black pin distillation of traditional glycerine forces heat exchange to be carried out outside the tower still, heating medium in the heat exchanger is a thermal oil, under vacuum-0.098MPa condition, the black pin of glycerine is heated up by thermal oil and the black pin heat exchange of glycerine, make in the black pin of glycerine the glycerine vaporization and from the top sucking-off of tower still, thereby obtain glycerine.The shortcoming of this distillation tower still is: the thermal oil temperature is higher, and the temperature instability, easily produces coking, curing in still-process, causes the obstruction of tower still and heat-exchanger pipeline, and etching apparatus reduces output.Glycerine at high temperature easily decomposes other organic impuritys such as producing aldehydes simultaneously, reduces the purity of gathering glycerine.
Summary of the invention
Main task of the present invention is to provide a kind of glycerine to deceive the pin distil process, specifically is a kind of employing vapor distillation technology, under the lower condition of temperature glycerine is become gas phase by liquid phase, thereby reaches effective separation, improves the yield of glycerine integral body.
For overcoming the above problems, the black pin distil process of a kind of glycerine of invention, isolate finished product glycerine and residue by the glycerine raw material through distillation tower, by the black pin still kettle of glycerine residue is separated once more then, reclaim the glycerine in the residue, at last to the glycerine of the separating processing of decolouring, generate finished product, it is characterized in that: described residue distillation is to carry out with steam distillation in the black pin still kettle of glycerine of sealing, the steps include: in the black pin still kettle of glycerine, to feed the steam of homo(io)thermism, and vacuumize simultaneously, guarantee that pressure is-0.098MPa, make glycerine under lower boiling state, become gas phase from liquid phase rapidly, reach effective isolating purpose.
Further, the steady temperature of described steam is 190-210 ℃.
Further, the lower boiling boiling point value of described glycerine is: 165---170 ℃.
The present invention also provides a kind of black pin still kettle of glycerine that realizes the black pin distil process of glycerine, main body is the tower still, have the glycerin vapor outlet at this tower still top, the bottom has slag notch, the sidewall of described tower still is provided with feed-pipe, its innovative point is: described tower still bottom is evenly distributed with the heating tube of some vertical direction, and described heating tube is connected with steam-pipe; Described feed-pipe stretches into and extends to the bottom of tower still from tower still middle part.
Further, described heating tube bottom is provided with the water storage bag, and the rising pipe of described water storage bag connects and composes circulation loop by heat exchanger and steam-pipe.
Further, the bottom of described tower still is connected with the reduced steam pipeline.
Further, the sidewall of described tower still is connected with the pipeline that purges steam.
The invention has the advantages that: adopt the vapor distillation technology,, make glycerine transfer gas phase to, form with black pin impurity and separate completely, increase glycerin extraction efficient, and make the yield of glycerine increase by 25% by liquid phase in conjunction with the black pin still kettle of glycerine.
Embodiment
Figure is the structural representation of the black pin still kettle of glycerine of the present invention.
Embodiment
The structure of the black pin still kettle of glycerine of the present invention comprises tower still 1, glycerin vapor outlet 2, slag notch 3, feed-pipe 4, heating tube 5, steam-pipe 6, water storage bag 7, heat exchanger 9, reduced steam pipeline 10, pipeline 11 purges steam as shown in Figure 1.
Above-mentioned tower still 1 top has the glycerin vapor outlet 2 that is connected with vacuum interface, and the bottom has slag notch 3, and sidewall is provided with feed-pipe 4, is provided with some heating tubes 5 that are connected with steam-pipe 6 in the cavity.The black pin raw material of glycerine can enter the inner chamber of tower still 1 from feed-pipe 4, described heating tube 5 vertically is evenly distributed on the bottom of tower still 1, superheated vapour enters in the heating tube 5 by steam-pipe 6, heat with the black pin of glycerine around the heating tube 5, make the glycerine in the black pin of glycerine at high temperature vaporize in the top of tower still 1, and exporting 2 vacuum sucking-offs by vertical glycerin vapor, the glycerine of vaporization collects through being condensed into liquid state.Because maintaining about 200 ℃ of the temperature-stable of steam prevents coking, the curing of the black pin of glycerine, avoids it attached on tower still 1 and the heating tube 5, the work-ing life of having improved heat transfer efficiency and equipment.The temperature of steam is higher than the boiling point of glycerine, and is lower than the polymeric reaction temperature of glycerine, has reduced the generation of the black pin polymerization glycerine in still-process of glycerine, has improved the yield of glycerine and the quality of product.
Described heating tube 5 bottoms are provided with water storage bag 7, and the rising pipe 8 of described water storage bag 7 connects and composes circulation loop by heat exchanger 9 and steam-pipe 6.After the steam cooling in the heating tube 5 becomes water of condensation, flow into water storage bag 7, the water of condensation in the water storage bag 7 becomes steam to enter in the heating tube 5 by steam-pipe 6 by in rising pipe 8 inflow heat exchangers 9 at heat exchanger 9 internal heating again.Steam was stored in the heating tube 5 before being condensed into water always, did not give off atmosphere, had made full use of the heat energy of steam, had improved the service efficiency of steam, cut down the consumption of energy.
The feed-pipe 4 of above-mentioned tower still 1 stretches into and extends to the bottom of tower still 1 from tower still 1 middle part.When having avoided the black pin of glycerine of normal temperature to enter tower still 1, expanded by heating, splash causes curing to the top of tower still, influences the work-ing life of equipment.
The bottom of tower still 1 is connected with reduced steam pipeline 10, is used to reduce the boiling point of the black pin of glycerine, makes that the glycerine in the black pin of glycerine is difficult for glycerol polymerization and decomposition reaction take place, and further improves the rate that makes of glycerine.Its principle is: the total pressure P in the tower still 1 equals the summation of glycerin vapor pressure P1 and water vapor pressure P2.In tower still 1, feed steam by reduced steam pipeline 10, and tower still 1 total pressure remains unchanged, thereby reduced the pressure of glycerin vapor, reach the purpose that reduces glycerine boiling point in the black pin of glycerine.
The sidewall of tower still 1 also is connected with the pipeline 11 that purges steam, and feeds steam by the pipeline 11 that purges steam in the black pin of glycerine of tower still 1 bottom, can reduce the viscosity of the black pin of glycerine, is convenient to the discharging of final residuum.
Glycerine disclosed by the invention is deceived the pin distil process, and its concrete steps are as follows:
At first, the glycerine raw material enters the glycerol distillation tower, at pressure be-0.098Mpa, temperature is to carry out glycerine under 170 ℃ the condition to separate, the finished product glycerine that separation is drawn enters finished product glycerine jar, the glycerine residue is that the black pin of glycerine enters the black pin still kettle of glycerine, and the glycerine in the glycerine residue is reclaimed further.
In the black pin still kettle of glycerine, employing be vapor distillation method.Promptly in the black pin still kettle of this glycerine, feed temperature and be 190-210 ℃ steam, the black pin isolation of this steam and glycerine; In the black pin still kettle of glycerine, tap into the pipeline that vacuumizes again, make its pressure be-0.098MPa; Acting as of this steam becomes gas phase with glycerine by liquid phase, and gasification rate is accelerated in acting as boiling point lowering of valve tube, fast gaseous state glycerine is separated from the outlet at still kettle top then.The cardinal principle of operating in this distillation tower just is: recently reach with solid residue and carry out isolating purpose in gaseous state, liquid different weight according to glycerine.This method is separation place glycerine effectively, guarantees the highest yield of glycerine.
In order to guarantee that the glycerine residue can access continuous uninterrupted and separate, the black pin still kettle of two glycerine in parallel in glycerol distillation tower exit, control by magnetic valve, make two glycerine deceive pin still kettle alternate feed, like this, when the black pin still kettle of a glycerine begins to react, second black pin still kettle of glycerine carried out charging, when the black pin still kettle of second glycerine began to react, the black pin still kettle of first glycerine had just in time just been reacted end, the beginning charging.By above-mentioned charging by turns, guaranteed that the extraction of the black pin of glycerine is continuous, save man-hour, raise the efficiency.
The glycerine of separating in the above-mentioned glycerine residue enters condenser after isolating from the top exit of the black pin still kettle of glycerine, enters the glycerine tundish after condensation under 30-50 ℃ the temperature, after handling through decolouring again, finished product.
Claims (8)
1. a glycerine is deceived the pin distil process, isolate finished product glycerine and residue by the glycerine raw material through distillation tower, by the black pin still kettle of glycerine residue is separated once more then, reclaim the glycerine in the residue, at last to the glycerine of the separating processing of decolouring, form finished product, it is characterized in that: described residue distillation is to carry out with steam distillation in the black pin still kettle of glycerine of sealing, the steps include: in the black pin still kettle of glycerine, to feed the steam of homo(io)thermism, and vacuumize simultaneously, guarantee that pressure is-0.098MPa to make glycerine become gas phase from liquid phase rapidly under lower boiling state, from being separated to the glycerine jar.
2. a kind of glycerine according to claim 1 is deceived the pin distil process, it is characterized in that: the steady temperature of described steam is 190-210 ℃.
3. a kind of glycerine according to claim 1 is deceived the pin distil process, it is characterized in that: the lower boiling boiling point value of described glycerine is: 165---170 ℃.
4. a glycerine of realizing the black pin distil process of the described glycerine of claim 1 is deceived the pin still kettle, main body is the tower still, have the glycerin vapor outlet at this tower still top, the bottom has slag notch, the sidewall of described tower still is provided with feed-pipe, it is characterized in that: described tower still bottom is provided with interchanger, and described interchanger is connected with steam-pipe; The described interchanger outside is provided with open reduced steam pipeline; Described feed-pipe stretches into and extends to the bottom of tower still from tower still middle part.
5. a kind of glycerine according to claim 4 is deceived pin distillation tower still, it is characterized in that: described interchanger vertically is located at tower still bottom by some independently enclosed heating tubes and constitutes.
6. a kind of glycerine according to claim 5 is deceived pin distillation tower still, it is characterized in that: described heating tube bottom is provided with the water storage bag, and the rising pipe of described water storage bag connects and composes circulation loop by heat exchanger and steam-pipe.
7. a kind of glycerine according to claim 4 is deceived pin distillation tower still, and it is characterized in that: the bottom of described tower still is connected with the reduced steam pipeline.
8. a kind of glycerine according to claim 4 is deceived pin distillation tower still, and it is characterized in that: the sidewall of described tower still is connected with the pipeline that purges steam.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910176881A CN101696155A (en) | 2009-09-23 | 2009-09-23 | Glycerol blackfoot distilling process and glycerol blackfoot distilling still for implementing same |
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| Application Number | Priority Date | Filing Date | Title |
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| CN200910176881A CN101696155A (en) | 2009-09-23 | 2009-09-23 | Glycerol blackfoot distilling process and glycerol blackfoot distilling still for implementing same |
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| CN101696155A true CN101696155A (en) | 2010-04-21 |
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| CN200910176881A Pending CN101696155A (en) | 2009-09-23 | 2009-09-23 | Glycerol blackfoot distilling process and glycerol blackfoot distilling still for implementing same |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775275A (en) * | 2012-09-06 | 2012-11-14 | 如皋市双马化工有限公司 | Refined glycerol purification process |
| CN103893986A (en) * | 2014-03-20 | 2014-07-02 | 攀钢集团攀枝花钢铁研究院有限公司 | Distillation method and detection method for organic components in flue gas desulfurization liquid |
| CN114225447A (en) * | 2021-12-17 | 2022-03-25 | 湖南道安环保科技有限公司 | Nitrogen heat-carrying sulfur vaporization device and process thereof |
-
2009
- 2009-09-23 CN CN200910176881A patent/CN101696155A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775275A (en) * | 2012-09-06 | 2012-11-14 | 如皋市双马化工有限公司 | Refined glycerol purification process |
| CN103893986A (en) * | 2014-03-20 | 2014-07-02 | 攀钢集团攀枝花钢铁研究院有限公司 | Distillation method and detection method for organic components in flue gas desulfurization liquid |
| CN114225447A (en) * | 2021-12-17 | 2022-03-25 | 湖南道安环保科技有限公司 | Nitrogen heat-carrying sulfur vaporization device and process thereof |
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Application publication date: 20100421 |