CN106831319B - Tetrachloroethylene purification and drying method - Google Patents
Tetrachloroethylene purification and drying method Download PDFInfo
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- CN106831319B CN106831319B CN201710055191.5A CN201710055191A CN106831319B CN 106831319 B CN106831319 B CN 106831319B CN 201710055191 A CN201710055191 A CN 201710055191A CN 106831319 B CN106831319 B CN 106831319B
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- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
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Abstract
The invention relates to a tetrachloroethylene purification and drying method, which comprises the following steps: 1) putting the tetrachloroethylene crude product flowing out of the rectifying tower and alkali liquor into an alkaline washing tank for mixing reaction to obtain a mixed material; 2) conveying the mixed material to an alkaline washing phase separator through an alkaline washing mixing pump for primary separation to obtain tetrachloroethylene and alkali liquor after primary separation; 3) carrying out secondary separation on the tetrachloroethylene subjected to the primary separation by using a high-efficiency phase separator to obtain tetrachloroethylene subjected to secondary separation; 4) and drying the tetrachloroethylene subjected to secondary separation in a dryer to obtain a tetrachloroethylene finished product. The pH value of the tetrachloroethylene finished product obtained by the method is 6-8, and the water content is 0-50 ppm, so that the application requirements are met.
Description
Technical Field
The invention relates to the field of production industry of tetrachloroethylene, and in particular relates to a tetrachloroethylene purification and drying method.
Background
After crude tetrachloroethylene is distilled out from the top of the rectifying tower, the main content of the crude tetrachloroethylene mainly reaches the national standard, but the components also contain HCl, and the HCl has higher tetrachloroethylene solubility. Tetrachloroethylene is used as a cleaning agent, has strict requirements on pH, has the pH value of 6-8, and cannot be used when the pH value is too high or too low; tetrachloroethylene is used as a raw material for producing the refrigerant R125, and has strict requirements on moisture, and the moisture content must be 0-50 ppm. Thus, tetrachloroethylene is a qualified product that is suitable for both industries, and must meet both moisture content and pH requirements.
The purification and drying process for producing tetrachloroethylene in the prior art is shown in figure 1: the tetrachloroethylene flowing out of the rectifying tower is contacted with alkali liquor in an inlet pipeline of an alkali washing mixing pump 2', the tetrachloroethylene and the alkali liquor are simply mixed by the alkali washing mixing pump 2', a part of mixed materials are returned from an outlet of the alkali washing mixing pump 2' to the inlet pipeline of the alkali washing mixing pump 2', and the other part of mixed materials are sent to an alkali washing phase separator 3 '; organic tetrachloroethylene and alkali liquor are separated, and the alkali liquor is used as waste alkali to be discharged; the organic tetrachloroethylene enters a dryer 5', and is dried by a primary dryer, a secondary dryer and a tertiary dryer, and finally, a tetrachloroethylene product is output.
The problems of the process are as follows: 1) the discharge of the rectifying tower cannot be stabilized at a constant value, so that the HCl cannot be completely removed in the neutralization process, and the pH is often too low; 2) after the organic matter is mixed with the alkali liquor, a large amount of water molecules are wrapped in the organic matter, so that the mixture of the organic matter and the alkali liquor can only be simply separated after entering a separator, tiny water particles in the organic matter cannot be removed, the water content of the separated organic matter is often more than 150ppm, and a large amount of solid alkali is dissolved after entering a dryer; 3) the obtained tetrachloroethylene product has more suspended matters, turbid appearance, water content of more than 50ppm, pH of more than 9 or pH of less than 5.
Disclosure of Invention
Accordingly, an object of the present invention is to provide a method for purifying and drying tetrachloroethylene, which can satisfy the application requirements of the pH and moisture of the tetrachloroethylene product.
The purpose of the invention is realized by the following technical scheme:
a tetrachloroethylene purification and drying method comprises the following steps:
s1: putting the tetrachloroethylene crude product flowing out of the rectifying tower and alkali liquor into an alkaline washing tank for mixing reaction to obtain a mixed material;
s2: conveying the mixed material to an alkaline washing phase separator through an alkaline washing mixing pump for primary separation to obtain tetrachloroethylene and alkali liquor after primary separation;
s3: carrying out secondary separation on the tetrachloroethylene subjected to the primary separation by using a high-efficiency phase separator to obtain tetrachloroethylene subjected to secondary separation;
s4: and drying the tetrachloroethylene subjected to secondary separation in a dryer to obtain a tetrachloroethylene finished product.
Compared with the prior art, the method has the advantages that the tetrachloroethylene and the alkali liquor are placed in the alkaline washing tank to be fully mixed, so that the sufficient volume ratio of the alkali liquor and the sufficient mixing time are ensured, and HCl in the tetrachloroethylene is fully neutralized; in addition, the tetrachloroethylene separated by the alkaline washing phase separator is continuously subjected to high-efficiency phase separation, so that the moisture content is further reduced; the pH value of the obtained tetrachloroethylene finished product is 6-8, the water content is 0-50 ppm, and the application requirements are met.
Further, in the step S1, the mass concentration of the alkali liquor is 5-10%. When the mass concentration of the alkali liquor is too low, the acid in the tetrachloroethylene cannot be sufficiently neutralized; when the mass concentration of the alkali liquor is too high, crystallization is easily caused at low temperature, and pipelines can be blocked in serious conditions.
Further, in the step S1, the volume ratio of the alkali liquor in the mixed material is 60-99%. In the alkaline washing stage, enough alkali liquor and tetrachloroethylene are required to be mixed so as to ensure that the pH value of the neutralized product is 6-8.
Further, the alkali liquor is sodium hydroxide solution. Because the sodium hydroxide has strong basicity and easy solubility, the sodium hydroxide solution is selected as the alkali liquor and is easy to carry out neutralization reaction with HCl in tetrachloroethylene so as to achieve the aim of removing acid.
Further, in the step S2, a part of the mixed material is conveyed to the caustic washing phase separator by the caustic washing mixing pump, and the other part of the mixed material is refluxed to the caustic washing tank by the caustic washing mixing pump. The part of mixed materials passing through the alkali washing mixing pump are used as reflux, the continuous back mixing of the materials is guaranteed, on one hand, tetrachloroethylene deposited at the bottom of the alkali washing tank is stirred and is fully mixed with alkali liquor, on the other hand, enough mixing time is guaranteed, and therefore HCl molecules in the tetrachloroethylene are fully neutralized.
Further, the flow of the mixed material which flows back to the alkaline washing tank from the alkaline washing mixing pump is 20-30 m3H is used as the reference value. Controlling the flow of the mixed material returned from the alkaline washing mixing pump to the alkaline washing tank to be 20-30 m3And h, not only is the back mixing of part of mixed materials realized, but also the sufficient amount of the mixed materials conveyed to the alkali washing phase separator is ensured, and the process cost is also considered.
Further, in the step S2, a part of the alkali liquor obtained after the primary separation is returned to the alkali washing tank, and the other part is discharged as waste alkali. And part of alkali liquor separated by the alkali washing phase separator flows back to the alkali washing tank for continuous reaction, so that the alkali liquor can be fully utilized.
Further, the flow of the alkali liquor which flows back to the alkali washing tank from the alkali washing phase separator is 40-50 m3H is used as the reference value. Controlling the flow of the alkali liquor which flows back to the alkali washing tank from the alkali washing phase separator to be 40-50 m3And h, ensuring that the volume ratio of the alkali liquor in the alkali washing tank is more than 60 percent, thereby ensuring that enough alkali liquor reacts with tetrachloroethylene.
Further, in step S3, the secondary separation process includes: after entering the high-efficiency phase separator, the tetrachloroethylene after primary separation sequentially passes through a feeding distributor, a liquid drop multiplication filler separation component and a special plate type phase separator component in the high-efficiency phase separator to carry out liquid drop multiplication separation. The water content of the tetrachloroethylene separated by the alkaline washing phase separator is high, and the water exists in the tetrachloroethylene in the form of very tiny particles, so that efficient phase separation is continuously carried out, and the water is secondarily separated in the liquid drop multiplication separation process, so that the water content of the tetrachloroethylene subjected to secondary separation is reduced to 0-80 ppm.
Further, in the step S4, the dryers include a primary dryer, a secondary dryer, and a tertiary dryer. And drying the tetrachloroethylene by a primary dryer, a secondary dryer and a tertiary dryer, and further reducing the moisture content to ensure that the moisture content of the final tetrachloroethylene finished product is 0-50 ppm so as to meet the application requirement.
For a better understanding and practice, the invention is described in detail below with reference to the accompanying drawings.
Drawings
FIG. 1 is a diagram of a conventional purification and drying process for tetrachloroethylene.
FIG. 2 is a schematic view of the tetrachloroethylene purification and drying process of example 1.
Detailed Description
Based on the problems existing in the prior art, the alkali liquor with the mass concentration of 10% and tetrachloroethylene are mixed for neutralization reaction, and the pH results measured after the reaction are shown in the following table 1 under different alkali liquor volume ratios and different working conditions:
TABLE 1 neutralization test results of alkali solution with tetrachloroethylene
Wherein, operating condition A, B, C specifically is respectively:
a: shaking for 5 times, and standing for 5 minutes;
b: shaking for 20 times, and standing for 30 minutes;
c: shake 20 times and rest for 30 minutes to replicate the test.
As can be seen from the test results in Table 1, to ensure that the pH of the product is acceptable during the neutralization stage in alkaline washing, the volume ratio of the alkaline solution is not less than 60%, and sufficient mixing time and standing time are ensured.
Therefore, the inventor researches the process again and provides a tetrachloroethylene purification and drying method, which comprises the steps of placing tetrachloroethylene and alkali liquor in an alkali washing tank for fully mixing, ensuring enough volume ratio of the alkali liquor and enough mixing time, and fully neutralizing acid in tetrachloroethylene; and the tetrachloroethylene after the alkaline washing phase separation is continuously subjected to high-efficiency phase separation, so that the moisture content is further reduced, and the pH value and the moisture content of the finally obtained tetrachloroethylene finished product both meet the application requirements. The following is further illustrated by specific examples.
Example 1
Please refer to fig. 2, which is a schematic diagram of the tetrachloroethylene purification and drying process of the present embodiment, the apparatus includes an alkaline washing tank 1, an alkaline washing mixing pump 2, an alkaline washing phase separator 3, a high efficiency phase separator 4, and a dryer 5.
The alkaline washing tank 1 comprises four alkaline washing tank inlets and an alkaline washing tank outlet 1e, wherein the four alkaline washing tank inlets are respectively an alkaline washing tank inlet 1a, an alkaline washing tank inlet 1b, an alkaline washing tank inlet 1c and an alkaline washing tank inlet 1 d.
The number of the alkali washing mixing pumps 2 is two, and the two alkali washing mixing pumps are respectively a first alkali washing mixing pump 21 and a second alkali washing mixing pump 22; the inlet 21a of the first alkali washing mixing pump and the inlet 22a of the second alkali washing mixing pump are both connected with the outlet 1e of the alkali washing tank; the outlet 21b of the first alkaline washing mixing pump is connected with the inlet 1d of the alkaline washing tank.
The alkaline washing phase separator 3 comprises an alkaline washing phase separator inlet 3a and two alkaline washing phase separator outlets, wherein the two alkaline washing phase separator outlets are an alkaline washing phase separator outlet 3b and an alkaline washing phase separator outlet 3c respectively; the inlet 3a of the alkaline washing phase separator is connected with the outlet 22b of the second alkaline washing mixing pump; the outlet 3b of the alkaline washing phase separator is divided into two paths, wherein one path is connected with the inlet 1c of the alkaline washing tank, and the other path is discharged outwards.
The high-efficiency phase separator 4 comprises a high-efficiency phase separator inlet 4a and two high-efficiency phase separator outlets, wherein the two high-efficiency phase separator outlets are a high-efficiency phase separator outlet 4b and a high-efficiency phase separator outlet 4c respectively; the inlet 4a of the high-efficiency phase separator is connected with the outlet 3c of the alkaline washing phase separator; the high-efficiency phase separator outlet 4b is discharged to the outside.
The dryer 5 is formed by connecting a primary dryer 51, a secondary dryer 52 and a tertiary dryer 53 in series; the inlet 5a of the dryer is connected with the outlet 4c of the high-efficiency phase separator; the dryer outlet 5b outputs the final tetrachloroethylene finished product.
Based on the above apparatus, the tetrachloroethylene purification and drying method of the embodiment specifically includes the following steps:
(1) tetrachloroethylene, fresh alkali liquor and part of alkali liquor which flows out of the rectifying tower and is separated by the alkali washing phase separator enter the alkali washing tank through an alkali washing tank inlet 1b, an alkali washing tank inlet 1a and an alkali washing tank inlet 1c respectively for mixing reaction to obtain a mixed material.
The alkali liquor of this example is preferably a 10% strength by mass sodium hydroxide solution. In order to make full use of the alkali liquor, part of the alkali liquor separated by the alkali washing phase separator flows back to the alkali washing tank for continuous reaction, so that the alkali liquor in the alkali washing tank comprises fresh alkali liquor and the alkali liquor overflowing back from the alkali washing phase separator. In order to ensure that tetrachloroethylene and enough alkali liquor perform a neutralization reaction in the alkali washing stage, in this embodiment, firstly, 80% of the liquid level of the alkali liquor is added into an alkali washing tank, and then, the flow rate of each material entering the alkali washing tank is controlled by using a flow valve, specifically, the flow rate of tetrachloroethylene flowing out of a rectifying tower entering the alkali washing tank through a distributor is 3m3The flow rate of fresh alkali liquor is 0.1-0.15 m3The flow rate of alkali liquor overflowing from the alkali washing phase separator is 40-50 m3And h, so that the volume ratio of the alkali liquor in the alkali washing tank is more than or equal to 60 percent.
(2) The mixed material is output from an outlet 1e of the alkaline washing tank and then enters an alkaline washing mixing pump 2; the mixed material output from the outlet 21b of the first alkaline washing mixed pump returns to the alkaline washing tank 1 through the inlet 1d of the alkaline washing tank; the mixed material output from the outlet 22b of the second alkali washing mixing pump enters the alkali washing phase separator 3 through the inlet 3a of the alkali washing phase separator for primary separation, and tetrachloroethylene and alkali liquor after primary separation are obtained.
This embodiment is in order to guarantee the dwell time of tetrachloroethylene in alkali lye the inside, takes out partial mixed material from the alkali wash mixing pump and returns to the alkali wash jar as the backward flow, has guaranteed the continuous backmixing of material like this to can let the deposit stir at the tetrachloroethylene who alkali wash tank bottom, carry out intensive mixing with alkali lye, thereby make the abundant neutralization of HCl molecule in the tetrachloroethylene fall, avoid the pH of product to hang down excessively. Specifically, the flow rate of the mixed material refluxed from the alkaline washing mixing pump in the embodiment is 20-30 m3And h, not only is the back mixing of part of mixed materials realized, but also the sufficient amount of the mixed materials conveyed to the alkali washing phase separator is ensured, and the process cost is also considered. The pH value of tetrachloroethylene after primary separation by an alkaline washing phase separator is 6-8, and the water content is 0-150 ppm.
(3) The alkali liquor after primary separation is output from an outlet 3b of the alkali washing phase separator, one part of the alkali liquor returns to the alkali washing tank 1 through an inlet 1c of the alkali washing tank, and the other part of the alkali liquor is discharged as waste alkali; the tetrachloroethylene after the primary separation is output from an outlet 3c of the alkaline washing phase separator, enters the high-efficiency phase separator 4 through an inlet 4a of the high-efficiency phase separator for secondary separation to obtain tetrachloroethylene after the secondary separation, and the water after the secondary separation is discharged through an outlet 4b of the high-efficiency phase separator.
Since the tetrachloroethylene after the primary separation in the alkaline washing phase separator has a relatively high moisture content and the moisture is present in the tetrachloroethylene as very fine particles, it is necessary to continue the high-efficiency phase separation process and separate the moisture for the second time.
The high efficiency phase separator of this example included a feed distributor, a droplet multiplication fiber packing separation module, a special plate pack type phase separator module, and a top reject phase separator. The secondary separation process comprises the following steps: the tetrachloroethylene after primary separation by the alkaline washing phase separator sequentially passes through a feeding distributor, a liquid drop multiplication fiber filler separation component and a special plate type phase separator component to carry out liquid drop multiplication separation. Specifically, tetrachloroethylene fluid carrying small moisture droplets enters a fiber bed with high porosity, and fibers in the fiber bed capture small aqueous phase droplets in an organic phase based on mechanisms such as direct interception, inertial collision, molecular diffusion and the like; the captured droplets are coalesced and grow on the surface of the fiber and move with the fluid to the downstream of the fiber bed; when the aqueous phase droplets increase to a certain particle size, the aqueous phase droplets are released on the downstream surface of the fiber bed due to the action of fluid drag and self gravity and enter the plate component along with the fluid; because the plate group has a large wet area, a stable flowing state and a vertical distance, a water phase can reach the surface of the plate in a short floating distance, water drops are coalesced by colliding with the surface of the plate, finally, water is formed, the water is discharged from the phase separator through the top, and the water content of tetrachloroethylene after secondary separation is 0-80 ppm.
(4) And the tetrachloroethylene after the secondary separation is output from an outlet 4c of the high-efficiency phase separator, enters a dryer 5 through an inlet 5a of the dryer for drying, and the tetrachloroethylene finished product is output from an outlet 5b of the dryer.
Specifically, the tetrachloroethylene after secondary separation is dried by a first-stage dryer 51, a second-stage dryer 52 and a third-stage dryer 53, so that the moisture content is further reduced, the pH of the final output tetrachloroethylene finished product is 6-8, and the moisture content is 0-50 ppm, so that the application requirements are met.
Compared with the prior art, the method has the advantages that the tetrachloroethylene and the alkali liquor are placed in the alkaline washing tank to be fully mixed, so that the sufficient volume ratio of the alkali liquor and the sufficient mixing time are ensured, and HCl in the tetrachloroethylene is fully neutralized; in addition, the tetrachloroethylene separated by the alkaline washing phase separator is continuously subjected to high-efficiency phase separation, so that the moisture content is further reduced; the pH value of the obtained tetrachloroethylene finished product is 6-8, the water content is 0-50 ppm, and the application requirements are met.
The above-mentioned embodiments only express one embodiment of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (9)
1. A tetrachloroethylene purification and drying method is characterized in that: the method comprises the following steps:
s1: putting tetrachloroethylene flowing out of a rectifying tower and alkali liquor into an alkaline washing tank for mixing reaction to obtain a mixed material; wherein the volume ratio of the alkali liquor in the mixed material is more than 60%, and the PH value of the obtained mixed material is 6-8;
s2: conveying the mixed material to an alkaline washing phase separator through an alkaline washing mixing pump for primary separation to obtain tetrachloroethylene and alkali liquor after primary separation;
s3: carrying out secondary moisture separation on the tetrachloroethylene subjected to the primary moisture separation by using a high-efficiency phase separator to obtain tetrachloroethylene subjected to secondary moisture separation;
s4: and drying the tetrachloroethylene subjected to secondary separation in a dryer to obtain a tetrachloroethylene product.
2. The purification and drying method for tetrachloroethylene according to claim 1, wherein: in the step S1, the mass concentration of the alkali liquor is 5-10%.
3. The purification and drying method for tetrachloroethylene according to claim 2, characterized in that: the alkali liquor is sodium hydroxide solution.
4. The purification and drying method for tetrachloroethylene according to claim 1, wherein: in the step S2, one part of the mixed material is conveyed to a caustic washing phase separator through a caustic washing mixing pump, and the other part of the mixed material flows back to a caustic washing tank through a caustic washing mixing pump.
5. The tetrachloroethylene purification and drying method according to claim 4, wherein the flow rate of the mixed material which flows back from the alkali washing mixing pump to the alkali washing tank is 20-30 m3/h。
6. The tetrachloroethylene purification and drying method according to claim 1 or 4, wherein: in the step S2, a part of the alkali solution obtained after the primary separation flows back to the alkali washing tank, and the other part is discharged as waste alkali.
7. The purification and drying method for tetrachloroethylene according to claim 6, wherein: the flow of the alkali liquor which flows back to the alkali washing tank from the alkali washing phase separator is 40-50 m3/h。
8. The method for purifying and drying tetrachloroethylene according to claim 1, wherein: in step S3, the secondary separation process includes: after entering the high-efficiency phase separator, the tetrachloroethylene after primary separation sequentially passes through a feeding distributor, a liquid drop multiplication filler separation component and a special plate type phase separator component in the high-efficiency phase separator to carry out liquid drop multiplication separation.
9. The purification and drying method for tetrachloroethylene according to claim 1, wherein: in the step S4, the dryers include a primary dryer, a secondary dryer, and a tertiary dryer.
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| CN110724030B (en) * | 2019-10-23 | 2022-08-19 | 成都市科隆化学品有限公司 | Method for producing environment-friendly grade tetrachloroethylene |
| CN112194560A (en) * | 2020-09-30 | 2021-01-08 | 宜宾海丰和锐有限公司 | Tetrachloroethylene purification method |
| CN112409127A (en) * | 2020-11-04 | 2021-02-26 | 宁波巨化化工科技有限公司 | Water removal method in tetrachloroethylene production process |
| CN115433057B (en) * | 2022-09-08 | 2023-12-22 | 嘉兴学院 | Method for recycling tetrachloroethylene in fur dry-cleaning waste |
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| GB1032442A (en) * | 1963-08-20 | 1966-06-08 | Sumitomo Chemical Co | Refining process for halogenated aliphatic hydrocarbons |
| US4932984A (en) * | 1989-07-27 | 1990-06-12 | The Dow Chemical Company | Process for reduction of chlorinated solvent emissions |
| JP2001181219A (en) * | 1999-12-28 | 2001-07-03 | Toagosei Co Ltd | Method for purifying chlorinated hydrocarbon |
| JP2008237988A (en) * | 2007-03-26 | 2008-10-09 | Toyobo Co Ltd | Regeneration method of organic solvent |
| CN202015517U (en) * | 2011-03-09 | 2011-10-26 | 上海安赐机械设备有限公司 | Composite high-efficiency phase separator |
| CN102557862B (en) * | 2012-01-11 | 2013-12-18 | 山东新龙科技股份有限公司 | Process for deoxidizing and dehydrating tetrachloroethylene and equipment for process |
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